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HCID 178472449, 화합물 → HCID 178472450, 화합물

HRID 1087972
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HRID 1087972 반응식
C([O:5][C:6](=[O:52])[CH:7]([CH:28]([C:30](=[O:51])[C@H:31]([CH2:36][CH2:37][CH2:38][CH2:39][NH:40][C:41]([O:43][CH2:44][C:45]1[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=1)=[O:42])[NH:32][C:33](=[O:35])[CH3:34])[NH2:29])[CH2:8][C:9]1([C:14](=[O:27])[NH:15][C@H:16]2[CH2:21][CH2:20][C@@H:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH2:18][CH2:17]2)[CH2:13][CH2:12][CH2:11][CH2:10]1)(C)(C)C>FC(F)(F)C(O)=O.ClCCl>[C:33]([NH:32][C@H:31]([C:30]([CH:28]([NH2:29])[CH:7]([CH2:8][C:9]1([C:14](=[O:27])[NH:15][C@H:16]2[CH2:21][CH2:20][C@@H:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])[CH2:18][CH2:17]2)[CH2:13][CH2:12][CH2:11][CH2:10]1)[C:6]([OH:52])=[O:5])=[O:51])[CH2:36][CH2:37][CH2:38][CH2:39][NH:40][C:41]([O:43][CH2:44][C:45]1[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=1)=[O:42])(=[O:35])[CH3:34]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 178472449HCID 178472449, 화합물

생성물 1

HCID 178472450HCID 178472450, 화합물수율 84%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

The t-butyl ester from Example 1 (571 mg, 0.783 mmol) was dissolved in a mixture of trifluoroacetic acid (2 ml) and dichloromethane (1 ml). The solution was kept at 4° C. overnight, then concentrated to dryness under vacuum, and the residue was azeotroped six times with dichloromethane. The resulting crude product was then taken up in ethyl acetate and washed with water until the washings were neutral. The organic phase was dried (MgSO4) and evaporated under vacuum to afford the title compound (442 mg, 84%) as a white foam. Found: C,61.89; H,7.76; N,7.93. C35H52N4O9 (0.5 H2O) requires C,61.65; H,7.69; N,8.22%.

후처리

  1. concentrationconcentrated to dryness under vacuum
  2. customthe residue was azeotroped six times with dichloromethane
  3. washwashed with water until the washings
  4. dry with materialThe organic phase was dried (MgSO4)
  5. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-6c84f8cdccd545919f4e3a985c54b87b
출처 데이터셋
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04960792

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