Allylamine → HCID 86737740, 화합물

HRID 476656

반응식

HRID 476656 반응식
[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]

참가 물질

4

반응물 2

HCID 7853AllylamineHCID 19972Mitomycin A

생성물 1

HCID 86737740HCID 86737740, 화합물수율 52.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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:

후처리

  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

출처 및 근거

ORD 기록
ord-16a35ad9e8e9478d83cb6cfa76ba86dc
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04885304

연결된 노트

불러오는 중…