Benzaldehyde → HCID 2825757、化合物

HRID 2218189ノート

反応式

HRID 2218189 の反応式
[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]

参加物

6

反応物 3

HCID 240BenzaldehydeHCID 5852PenicillamineHCID 7918Acetic Anhydride

生成物 1

HCID 2825757HCID 2825757、化合物収率 89.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-690403936317446380878c020bbce5d9
出典データセット
uspto-grants-2008_08
特許番号
US07410987B2

反応ノート

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