ChemicalBook CAS DataBase List N-Benzylhydroxylamine hydrochloride

N-Benzylhydroxylamine hydrochloride synthesis

9synthesis methods

Product Name:N-Benzylhydroxylamine hydrochloride
CAS Number:29601-98-7
Molecular formula:C7H10ClNO
Molecular Weight:159.61

57079-14-8 Synthesis

(Z)-6-(3-Carboxyacrylamido)hexanoic acid

57079-14-8
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29601-98-7
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Yield:29601-98-7 87.3%

Reaction Conditions:

with hydroxylamine hydrochloride in ethanol;tert-butyl methyl ether at 35; for 3 h;

Steps:

1.2 Step 2: Synthesis of N-benzylhydroxylamine hydrochloride

Take a 5L three-necked bottle, install a thermometer, and stir mechanically.Add C-phenyl-N-benzylnitrone (535.7g, content 98.0%, 2.46mol),Add ethanol (197.3g, 4.28mol),Add methyl tert-butyl ether (1849.9g, 20.98mol),Warm up to 35°C, stir to dissolve,Add hydroxylamine hydrochloride (182.9g, 2.63mol),The reaction was kept at 35°C for 3 hours, and the C-phenyl-N benzyl nitrone was controlled to be ≤2.0%.Cool down to 0, keep for 2 hours to crystallize,Filter, wash the filter cake with methyl tert-butyl ether,The crude N-benzylhydroxylamine hydrochloride was obtained.Take another 2L three-necked bottle, install a thermometer, and stir mechanically.Add crude N-benzyl hydroxylamine hydrochloride,Add dichloromethane (2195.6g, 25.85mol),25 heat preservation and beating for 2 hours,Filter, wash the filter cake with dichloromethane, dry,Obtain N-benzylhydroxylamine hydrochloride (343.2g, 2.15mol),The yield was 87.3%, and the purity was 99.53%.

References:

CN113292446,2021,A Location in patent:Paragraph 0076; 0078; 0083-0086

103-49-1 Synthesis