Trifluoroacetic acid → HCID 67609530, 화합물

HRID 1965191노트

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HRID 1965191 반응식
C(OC([N:8]1[CH2:12][CH:11]([O:13][CH2:14][C:15]2[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=2)[CH:10]2[N:22]([C:25](=[O:48])[CH:26]([NH:31][C:32](=[O:47])[CH:33]([N:35]([C:37]([O:39][CH2:40][C:41]3[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=3)=[O:38])[CH3:36])[CH3:34])[C:27]([CH3:30])([CH3:29])[CH3:28])[CH2:23][CH2:24][CH:9]12)=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH2:40]([O:39][C:37](=[O:38])[N:35]([CH:33]([C:32](=[O:47])[NH:31][CH:26]([C:25]([N:22]1[CH2:23][CH2:24][CH:9]2[NH:8][CH2:12][CH:11]([O:13][CH2:14][C:15]3[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=3)[CH:10]12)=[O:48])[C:27]([CH3:28])([CH3:30])[CH3:29])[CH3:34])[CH3:36])[C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 67606700HCID 67606700, 화합물

생성물 1

HCID 67609530HCID 67609530, 화합물수율 97%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

A solution containing 48 (4.0 g, 5.98 mmol) in DCM (20 mL) was cooled to 0° C. and TFA (10 mL) was added. After 2.5 h, the reaction mixture was concentrated in vacuo and the residue was dissolved in EtOAc. The organic solution was washed successively with aqueous NaHCO3, water, and brine, dried over anhydrous Na2SO4, filtered, and concentrated to afford 3.3 g of 49 as a beige-colored foam which was used directly in the next reaction. Mass spectrum, m/z [569.1] (M+Na)+.

후처리

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. dissolutionthe residue was dissolved in EtOAc
  3. washThe organic solution was washed successively with aqueous NaHCO3, water, and brine
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c5bdb9f1d84947649bf0829664ff53d4
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08415486B2

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