Methanol → HCID 86737736、化合物

HRID 476652

反応式

HRID 476652 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.[CH3:26][OH:27]>C(N)C1OC=CC=1>[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:10][CH2:7][C:6]3[O:27][CH:26]=[CH:3][CH:4]=3)=[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 887MethanolHCID 19972Mitomycin A

生成物 1

HCID 86737736HCID 86737736、化合物収率 42.7%

試薬・触媒・溶媒 1

HCID 3438Furfurylamine溶媒

実験手順

To a solution of 60 mg (0.17 mmol) of mitomycin A in 8 ml of anhydrous methanol, 0.5 ml of furfurylamine was added with stirring. The progress of the reaction was periodically checked by TLC and the reaction appeared to be complete in 3 hours. The solvent was removed by evaporation under reduced pressure and the residue was chromatographed using silica-gel as adsorbent. The fraction obtained by eluting the column with ethyl acetate was evaporated. Recrystallization from a mixture of chloroform and hexane gave 30 mg (42.7% yield) of the desired product as purple-colored crystals having a melting point of 62°-63° (decomposing) and providing the following analysis:

後処理

  1. customThe solvent was removed by evaporation under reduced pressure
  2. customthe residue was chromatographed
  3. customThe fraction obtained
  4. washby eluting the column with ethyl acetate
  5. customwas evaporated
  6. customRecrystallization
  7. additionfrom a mixture of chloroform and hexane

出典と根拠

ORDレコード
ord-6695317cff2e4ca1939b1de3423387a9
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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