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Mitomycin F → HCID 88629851、化合物

HRID 476663
ノート
印刷プレビュー

反応式

HRID 476663 の反応式
[CH3:1][C:2]1[C:8](=[O:9])[C:7]2[N:10]3[C@@:14](OC)([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[N:23]([CH3:24])[C@H:12]1[CH2:11]3.[C:27]([O-])(=O)C.[Na+].Cl.[OH:33][CH2:34][CH2:35][CH2:36][NH2:37]>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:37][CH2:36][CH2:35][CH2:34][OH:33])=[C:2]([CH3:1])[C:8](=[O:9])[C:7]=2[N:10]2[CH2:11][CH:12]3[N:23]([CH3:24])[CH:13]3[C:14]12[CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 159845Mitomycin FHCID 517045Sodium AcetateHCID 30148263-Amino-1-propanol hydrochloride

生成物 1

HCID 88629851HCID 88629851、化合物収率 61%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

実験手順

To a solution of 50 mg (0.13 mmol) of N-methylmitomycin A in 10 ml of anhydrous methanol, a solution of 82 mg (1 mmol) sodium acetate in 2.5 ml of methanol and a solution of 130 mg (1 mmol) of 3-hydroxypropylamine hydrochloride in 2.5 ml of methanol were added alternatively with vigorous stirring, over a period of 10 minutes. The progress of the stirred reaction was checked frequently by TLC and appeared to be complete in 24 hours. The solvent was evaporated 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 methylene chloride and hexane gave 31 mg. (61% yield) of the desired product as purple-colored crystals having a melting point of 139°-140° (decomposing) and providing the following analysis:

後処理

  1. customThe progress of the stirred reaction
  2. customThe solvent was evaporated under reduced pressure
  3. customthe residue was chromatographed
  4. customThe fraction obtained
  5. washby eluting the column with ethyl acetate
  6. customwas evaporated
  7. customRecrystallization
  8. additionfrom a mixture of methylene chloride and hexane
  9. customgave 31 mg

出典と根拠

ORDレコード
ord-a97766e0d2cf4d0aa9bce7fe6a4dd051
出典データセット
uspto-grants-1989_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04885304

反応ノート

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