Allylamine → HCID 86737740、化合物

HRID 476656

反応式

HRID 476656 の反応式
[CH3:1][C:2]1[C:8](=[O:9])[C:7]2[N:10]3[C@@:14]([O:21][CH3:22])([C@H:15]([CH2:16][O:17][C:18]([NH2:20])=[O:19])[C:6]=2[C:4](=[O:5])[C:3]=1OC)[C@H:13]1[NH:23][C@H:12]1[CH2:11]3.[CH2:26]([NH2:29])[CH:27]=[CH2:28]>CO>[C:18](=[O:17])([OH:19])[NH2:20].[OH:17][CH2:16][CH:15]1[C:6]2[C:4](=[O:5])[C:3]([NH:29][CH2:26][CH:27]=[CH2:28])=[C:2]([CH3:1])[C:8](=[O:9])[C:7]=2[N:10]2[CH2:11][CH:12]3[NH:23][CH:13]3[C:14]12[O:21][CH3:22]

参加物

4

反応物 2

HCID 7853AllylamineHCID 19972Mitomycin A

生成物 1

HCID 86737740HCID 86737740、化合物収率 52.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 100 mg (0.28 mmol) of mitomycin A in 8 ml of anhydrous methanol, 150 mg (2.6 mmol) of allylamine was added with constant stirring. The reaction mixture was stirred overnight whereupon TLC indicated the absence of starting material. The solvent was then evaporated under reduced pressure and the residue was chromatographed using silica-gel as adsorbent. The fraction obtained by eluting the column from ethyl acetate was evaporated under reduced pressure. Recrystallization from a mixture of methylene chloride and hexane gave 29 mg (27.0% yield) of the desired product as purple-colored crystals having a melting point of 81°-82° (decomposing) and providing the following analysis:

後処理

  1. customThe solvent was then evaporated under reduced pressure
  2. customthe residue was chromatographed
  3. customThe fraction obtained
  4. washby eluting the column from ethyl acetate
  5. customwas evaporated under reduced pressure
  6. customRecrystallization
  7. additionfrom a mixture of methylene chloride and hexane

出典と根拠

ORDレコード
ord-16a35ad9e8e9478d83cb6cfa76ba86dc
出典データセット
uspto-grants-1989_12
特許番号
US04885304

関連ノート

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