* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
196 g (2.2 moles) of N-methylglycine was dissolved in 360 g of water, heated to 80C, and the hot solution was quickly added to the above S-carboxymethylisothiourea aqueous solution to keep the temperature of the reaction system at not lower than 60 ° C. The reaction was stirred for 3 hours. The heating was stopped. The system was cooled to 0-5 ° C in an ice-water bath. The filter cake was washed with a small amount of absolute ethanol and dried to give 238 g of white crystals, melting at 294 ° C. Acid, yield 80percent.The filtrate was extracted four times with 300 ml of chloroform, and the extracts were combined. The chloroform was recovered at normal pressure and the residue was distilled under reduced pressure (vacuum 0.098 MPa). The fractions were collected at 104-106 ° C to give 156 g of thioglycolic acid in a yield of 85percent, and 156 g
Reference：
[1] Patent: CN105777594, 2016, A, . Location in patent: Paragraph 0025; 0026
2
[ 107-97-1 ]
[ 496-72-0 ]
[ 887571-32-6 ]
Reference：
[1] Asian Journal of Chemistry, 2014, vol. 26, # 3, p. 926 - 932
(3R*,3'R*,4'S*)-5,7-dibromo-1'-methyl-3'-nitro-4'-(trifluoromethyl)spiro[indoline-3,2'-pyrrolidin]-2-one[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
66%
In isopropyl alcohol; for 48h;Reflux;
General procedure: 4.2. General procedure for the preparation of spiro[indoline-3,20-pyrrolidin]-2-ones 3 and spiro[indoline-3,30-pyrrolizin]-2-ones 4 and 6 A mixture of corresponding isatin 2 (1.0 mmol) and sarcosine(0.13 g, 1.5 mmol) or proline (0.17 g, 1.5 mmol) was stirred in isopropanol (4 mL), and corresponding nitroalkene 1 (1.0 mmol)was added in one portion. The resulting mixture was stirred atreux for 48 h and the reaction progress was monitored by TLC.Upon completion, the mixture was diluted with brine (10 mL),resulting precipitate was ltered off and washed with water andhexane and vacuum dried. In some cases, additional recrystallisa-tion from the mixture hexane/CH2Cl2 (2:1) was necessary.
5'-(4-bromophenyl)-2'-methyl-2',3',3a',6a'-tetrahydro-4'H-spiro[indene-2,1'-pyrrolo[3,4-c]pyrrole]-1,3,4',6'(5'H)-tetraone[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
84%
In methanol; at 100℃; under 750.075 Torr;Microwave irradiation;
General procedure: A mixture of respective 3-(4- 1-(aryl/alkyl)-1H-pyrrole-2,5-dione (1 mmol), ninhydrin (1 mmol) and sarcosine in methanol was placed in a microwave synthesizer. The vial was subjected to microwave irradiation programmed at 100 C, 120W and 1 bar pressure. After completion of the reaction (TLC), the solvent was removed and the product was purified by column chromatography using petroleum ether-ethyl acetate mixture (4:1 v/v) as eluent to obtain pure cycloadduct 4.
5'-benzyl-2'-methyl-2',3',3a',6a'-tetrahydro-4'H-spiro[indene-2,1'-pyrrolo[3,4-c]pyrrole]-1,3,4',6'(5'H)-tetraone[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
82%
In methanol; at 100℃; under 750.075 Torr;Microwave irradiation;
General procedure: A mixture of respective 3-(4- 1-(aryl/alkyl)-1H-pyrrole-2,5-dione (1 mmol), ninhydrin (1 mmol) and sarcosine in methanol was placed in a microwave synthesizer. The vial was subjected to microwave irradiation programmed at 100 C, 120W and 1 bar pressure. After completion of the reaction (TLC), the solvent was removed and the product was purified by column chromatography using petroleum ether-ethyl acetate mixture (4:1 v/v) as eluent to obtain pure cycloadduct 4.
With phosphotungstic acid; In ethanol; at 80℃; for 6h;
Accurately weighed 4,6-dichloro isatin (0.56 g),Sarcosine (0.25 g)Was added to a 100 mL flask,Add about 50mL ethanol solvent,Dropwise pulegone (0.3 g).The reaction was carried out under conditions catalyzed by phosphotungstic acid (0.5 g), heated to 80 C with a heat jacket,Placed on a magnetic stirrer,Reflux reaction for 6 hours,The reaction solution was concentrated by rotary steam and then filtered,The obtained filter cake was recrystallized by adding 50 ml of a mixed solution of ethyl acetate and petroleum ether 1: 1,A pale yellow crystalline powder (0.57 g)The overall yield was 72.6%.
5'-(3-chloro-4-methoxyphenyl)-1',1'',3''-trimethyl-2''H-dispiro[indene-2,2'-pyrrolidine-4',5''-pyrimidine]-1,2'',3,4'',6''(1''H,3''H)-pentaone[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
75%
With magnesium silicate; In ethanol; at 120℃; under 1500.15 Torr; for 1h;Microwave irradiation;
General procedure: To a solution of biphenyl carboxaldehyde 1d (0.1 g, 0.54 mmol) in ethanol (1.5 mL) was added N, N-dimethyl barbituric acid, 4 (0.1 g, 0.64 mmol), ninhydrin, 2 (0.1 g, 1.0 mmol), sarcosine, 3 (57 mg, 0.64 mmol) and magnesium silicate catalyst (10 mol%) at room temperature. The reaction mass was irradiated by microwave irradiations in a Microwave Vials 0.2-0.5mL of Biotage Initiator at 120 C, 300 W, 2 bar reactionpressure for 90 min and until the completion of starting material. The title compound was precipitated as yellow solid on standing the reaction mass. Then it was filtered and washed with cold methanol to remove polar impurities. The compound was further recrystallized using dichloromethane:methanol: tetrahydrofuran (3:1:1) to get 88% yield as colorless prisms.
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