Trifluoroacetic acid methylene chloride → HCID 23554372, 화합물

HRID 433451노트

반응식

HRID 433451 반응식
C(OC([NH:8][C@H:9]([C:11]([NH:13][CH:14]1[N:20]=[C:19]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:18]2[CH:27]=[CH:28][CH:29]=[CH:30][C:17]=2[N:16]([CH2:31][CH2:32][CH2:33][C:34]([F:37])([F:36])[F:35])[C:15]1=[O:38])=[O:12])[CH3:10])=O)(C)(C)C.C(O)(C(F)(F)F)=O.C(Cl)Cl>>[NH2:8][C@H:9]([C:11]([NH:13][CH:14]1[N:20]=[C:19]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:18]2[CH:27]=[CH:28][CH:29]=[CH:30][C:17]=2[N:16]([CH2:31][CH2:32][CH2:33][C:34]([F:37])([F:35])[F:36])[C:15]1=[O:38])=[O:12])[CH3:10]

참가 물질

3

반응물 2

HCID 21863450Trifluoroacetic acid methylene chlorideHCID 23554393HCID 23554393, 화합물

생성물 1

HCID 23554372HCID 23554372, 화합물수율 68.3%

실험 절차

3-(N′-(tert-Butoxycarbonyl)-L-alaninyl)amino-2,3-dihydro-1-(4,4,4-trifluorobutyl)-5-phenyl-1H-1,4-benzodiazepin-2-one (1.21 g, 2.27 mmol) was added to 50 mL of a stirring solution of 15% TFA/methylene chloride in one portion. After stirring 2 h, the reaction mixture was concentrated under reduced pressure and the residue was dissolved in 100 mL of methylene chloride. This solution was washed twice with saturated sodium bicarbonate, once with brine and then dried over sodium sulfate. Purification of the crude product using silica gel column chromatography (1-5% methanol/methylene chloride) gave 670 mg (68%) of a light pink foam.

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in 100 mL of methylene chloride
  3. washThis solution was washed twice with saturated sodium bicarbonate, once with brine
  4. dry with materialdried over sodium sulfate
  5. customPurification of the crude product

출처 및 근거

ORD 기록
ord-7db86ae15b214f6e9a8b79713f7d87e7
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06667305B1

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