Trichloroacetic Acid → 97139-59-8

HRID 2290841ノート

反応式

HRID 2290841 の反応式
[CH2:1]([NH:8][C:9](=[O:12])[NH:10][OH:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClC(Cl)(Cl)C(O)=O.[CH2:20]1[CH:26](O)[NH:25][P:23]([N:28]([CH2:32][CH2:33][Cl:34])[CH2:29][CH2:30][Cl:31])(=[O:24])[O:22][CH2:21]1>CC(C)=O.C(Cl)Cl>[CH2:1]([NH:8][C:9](=[O:12])[N:10]([OH:11])[CH:26]1[CH2:20][CH2:21][O:22][P:23]([N:28]([CH2:32][CH2:33][Cl:34])[CH2:29][CH2:30][Cl:31])(=[O:24])[NH:25]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 3

HCID 6421Trichloroacetic AcidHCID 997354-HydroxycyclophosphamideHCID 13770898N-Benzyl-N'-hydroxyurea

生成物 1

HCID 1377089997139-59-8

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 6344Dichloromethane溶媒

実験手順

540 mg (3.25 mmol) of 3-benzyl-1-hydroxyurea in 40 ml of acetone and a catalytic amount of trichloroacetic acid were added to 900 mg (3.25 mmol) of 4-hydroxycyclophosphamide in 1 ml of methylenechloride. The mixture was stored overnight at -25° C., the crystals were then drawn off by suction, washed with acetone and ether and recrystallized from ethyl acetate.

後処理

  1. washwashed with acetone and ether
  2. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-98245b4734e949f4abb48ec7ade04ca1
出典データセット
uspto-grants-1986_10
特許番号
US04618692

反応ノート

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