ChemicalBook CAS DataBase List Pramipexole impurity 7

Pramipexole impurity 7 synthesis

10synthesis methods

Product Name:Pramipexole impurity 7
CAS Number:106092-09-5
Molecular formula:C7H11N3S
Molecular Weight:169.25

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106092-09-5
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Yield:106092-09-5 92%

Reaction Conditions:

Stage #1:(S)-4,5,6,7-tetrahydro-benzothiazole-2,6-diamine tartrate trihydrate with water;pyrographite at 80; for 1 h;
Stage #2: with water;potassium hydroxide;sodium hydroxide; pH=12 at 10 - 20; for 0.5 h;Temperature;

Steps:

1A-7A; 1B-3B Example 4A
Add (S) -2,6-diamino-4,5,6,7-tetrahydrobenzothiazole * L-tartrate (0.156mol, 50g), 100ml water to the reaction vessel,Heat to 80 ° C, completely dissolve, add 2 grams of activated carbon and stir for 1 hour.Filtered, and the filtrate was cooled to between 10 ° C and 20 ° C,Add 15% (mass ratio) aqueous solution of sodium hydroxide and potassium hydroxide (NaOH molar amount: KOH molar amount = 1: 1),Until pH = 12.0, a precipitate is precipitated, and stirring is continued for 30 min.Filtration, an appropriate amount of ice water lotion, and drying to obtain 24.3 g of off-white solid, yield 92%,Ignition residue 0.2%, content ≧ 99.5%, single impurity ≦ 0.1%.

References:

Fujian Furui Mingde Pharmaceutical Co., Ltd.;Ren Jianqiang;Zhang Guozu;Zhang Tao;Huang Jianlong CN110669024, 2020, A Location in patent:Paragraph 0023-0042

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