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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Trifluoroacetic acid → HCID 86754241, 화합물

HRID 582488
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HRID 582488 반응식
C([O:14][C:15]([C:17]1[N:18]2[C@H:21]([S:22][CH2:23][C:24]=1/[CH:25]=[C:26]1/[C:27](=[O:35])[N:28]([CH2:31][CH:32]([CH3:34])[CH3:33])[CH2:29][CH2:30]/1)[C@H:20]([NH:36]C(OC(C)(C)C)=O)[C:19]2=[O:44])=[O:16])(C1C=CC=CC=1)C1C=CC=CC=1.[F:45][C:46]([F:51])([F:50])[C:47]([OH:49])=[O:48]>ClCCl.C1(OC)C=CC=CC=1>[F:45][C:46]([F:51])([F:50])[C:47]([OH:49])=[O:48].[NH2:36][C@@H:20]1[C:19](=[O:44])[N:18]2[C@@H:21]1[S:22][CH2:23][C:24](/[CH:25]=[C:26]1/[C:27](=[O:35])[N:28]([CH2:31][CH:32]([CH3:33])[CH3:34])[CH2:29][CH2:30]/1)=[C:17]2[C:15]([OH:16])=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 6422Trifluoroacetic acidHCID 86754243HCID 86754243, 화합물

생성물 1

HCID 86754241HCID 86754241, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 7519Anisole용매

실험 절차

(E)-(6R,7R)-7-tert-Butoxycarbonylamino-3-(1-isobutyl-2-oxo-pyrrolidin-3-ylidenemethyl)-8-oxo-5-thia-1-aza-bicyclo[4.2.0]oct-2-ene-2-carboxylic acid benzhydryl ester (21.9 g, 35.0 mmol) was dissolved in 240 ml dichloromethane and 23 ml anisole. At 20° C. 120 ml trifluoroacetic acid were added dropwise while maintaining the temperature below 50° C. After complete addition the ice-bath was removed and the solution was stirred at ambient temperature for 2.5 hours The volatile material was then removed under reduced pressure and the remaining yellow oil was added slowly to 400 ml of diethyl ether, in which the product started to precipitate. After 1.5 hours the suspension was filtered under argon atmosphere and the remaining crystals were stirred in 150 ml of ethyl acetate for 2 hours. The suspension was filtered under argon giving the desired product as a yellow crystalline powder.

후처리

  1. customAt 20° C
  2. temperaturewhile maintaining the temperature below 50° C
  3. customwas removed
  4. customwas then removed under reduced pressure
  5. additionthe remaining yellow oil was added slowly to 400 ml of diethyl ether, in which the product
  6. customto precipitate
  7. filtrationAfter 1.5 hours the suspension was filtered under argon atmosphere
  8. stirringthe remaining crystals were stirred in 150 ml of ethyl acetate for 2 hours
  9. filtrationThe suspension was filtered under argon giving the desired product as a yellow crystalline powder

출처 및 근거

ORD 기록
ord-f12a858473fa47849d9502d559d39477
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05925632

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