Sodium borohydride → 2-hydroxymethylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one

HRID 1281886노트

반응식

HRID 1281886 반응식
[CH:1]([C:3]1[S:17][C:6]2[O:7][C:8]3[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=3[NH:10][C:11](=[O:12])[C:5]=2[CH:4]=1)=[O:2].[BH4-].[Na+]>CO.O>[OH:2][CH2:1][C:3]1[S:17][C:6]2[O:7][C:8]3[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=3[NH:10][C:11](=[O:12])[C:5]=2[CH:4]=1

참가 물질

5

반응물 2

HCID 4311764Sodium borohydrideHCID 184221402-Formylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one

생성물 1

HCID 184221522-hydroxymethylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one수율 62%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

2-Formylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.6 g) was suspended in methanol (30 ml) and sodium borohydride (480 mg) was added. The mixture was stirred at room temperature for 1.5 hours. The reaction mixture was diluted with water and extracted 3 times with chloroform. The organic layer was dried over sodium sulfate and the solvent was evaporated under reduced pressure. To the residue were added chloroform and diisopropyl ether and the precipitated crystals were collected by filtration to give 2-hydroxymethylthieno[2,3-b][1,5]benzoxazepin-4(5H)-one (1.0 g).

후처리

  1. extractionextracted 3 times with chloroform
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. additionTo the residue were added chloroform and diisopropyl ether
  5. filtrationthe precipitated crystals were collected by filtration

출처 및 근거

ORD 기록
ord-bbae3245b4314f84ae17d176b46eac19
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06455521B1

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