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5-oxo-6H-benzo[b][1]benzothiepine-2-carboxylic acid → 10,11-Dihydro-11-hydroxydibenzo[b,f]thiepin-3-carboxylic Acid

HRID 485421
노트
인쇄 미리보기

반응식

HRID 485421 반응식
[O:1]=[C:2]1[CH2:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[S:5][C:4]2[CH:13]=[C:14]([C:17]([OH:19])=[O:18])[CH:15]=[CH:16][C:3]1=2.[BH4-].[Na+]>C(=O)(O)[O-].[Na+]>[OH:1][CH:2]1[CH2:8][C:7]2[CH:9]=[CH:10][CH:11]=[CH:12][C:6]=2[S:5][C:4]2[CH:13]=[C:14]([C:17]([OH:19])=[O:18])[CH:15]=[CH:16][C:3]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8270515-oxo-6H-benzo[b][1]benzothiepine-2-carboxylic acidHCID 4311764Sodium borohydride

생성물 1

HCID 1315185610,11-Dihydro-11-hydroxydibenzo[b,f]thiepin-3-carboxylic Acid수율 96.2%

시약·촉매·용매 1

HCID 516892Sodium Bicarbonate용매

실험 절차

16.3 G. 10,11-dihydro-11-oxodibenzo-[b,f]thiepin-3-carboxylic acid is stirred in aqueous sodium bicarbonate solution and 5 g. sodium borohydride is added in portions. The foaming mixture is stirred for an additional half hour. The solution is extracted with ether and the aqueous layer acidified with hydrochloric acid and the solid filtered and dried to yield 15.8 g. of the desired yellow solid (96.2% yield), m.p. 202°-204° C.

후처리

  1. extractionThe solution is extracted with ether
  2. filtrationthe solid filtered
  3. customdried
  4. customto yield 15.8 g

출처 및 근거

ORD 기록
ord-bd4a1abf95c9446891f8581486798769
출처 데이터셋
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04536507

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