Benzaldehyde → HCID 2825757, 화합물

HRID 2216430노트

반응식

HRID 2216430 반응식
[CH:1](=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:9][C@@H:10]([C:15]([OH:17])=[O:16])[C:11]([SH:14])([CH3:13])[CH3:12].[C:18](OC(=O)C)(=[O:20])[CH3:19]>C(O)C.O>[C:18]([N:9]1[C@@H:10]([C:15]([OH:17])=[O:16])[C:11]([CH3:13])([CH3:12])[S:14][C@H:1]1[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)(=[O:20])[CH3:19]

참가 물질

6

반응물 3

HCID 240BenzaldehydeHCID 5852PenicillamineHCID 7918Acetic Anhydride

생성물 1

HCID 2825757HCID 2825757, 화합물수율 89.4%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

A solution of benzaldehyde (102 ml, 1.01 mol) in ethanol (300 ml) was added to a solution of D-penicillamine (150 g, 1.01 mol) in water (900 ml) at room temperature. The mixture was stirred at room temperature for 15 minutes and under ice-cooling for 1.5 hours, and then the precipitated crystals were filtered off and dried. Acetic anhydride (480 ml, 5.05 mol) was added dropwise to a solution of the obtained crystals in water (700 ml) at 60° C. over 15 minutes. The mixture was stirred at the temperature for 15 minutes, then at room temperature for 15 minutes and under ice-cooling for 1.5 hours, and the precipitated crystals were filtered off and dried to give 252.3 g (89%) of the target compound.

후처리

  1. temperaturecooling for 1.5 hours
  2. filtrationthe precipitated crystals were filtered off
  3. customdried
  4. stirringThe mixture was stirred at the temperature for 15 minutes
  5. waitat room temperature for 15 minutes
  6. temperatureunder ice-cooling for 1.5 hours
  7. filtrationthe precipitated crystals were filtered off
  8. customdried

출처 및 근거

ORD 기록
ord-0a3be4f3e20c49189335732640fc5dc6
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07112598B2

반응 노트

불러오는 중…