Acetic Anhydride → HCID 66779757, 화합물

HRID 712571노트

반응식

HRID 712571 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:10]([C:11]3[CH:18]=[CH:17][C:14]([CH2:15][NH2:16])=[CH:13][CH:12]=3)=[CH:9][N:8]([S:19]([C:22]3[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][CH:23]=3)(=[O:21])=[O:20])[C:5]2=[N:6][CH:7]=1.C(N(CC)CC)C.[C:36](OC(=O)C)(=[O:38])[CH3:37].CCOC(C)=O>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]2[C:10]([C:11]3[CH:12]=[CH:13][C:14]([CH2:15][NH:16][C:36](=[O:38])[CH3:37])=[CH:17][CH:18]=3)=[CH:9][N:8]([S:19]([C:22]3[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][CH:23]=3)(=[O:20])=[O:21])[C:5]2=[N:6][CH:7]=1

참가 물질

6

반응물 4

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 667783594-[5-bromo-1-(toluene-4-sulfonyl)-1H-pyrrolo[2,3-b]pyridin-3-yl]-benzylamine

생성물 1

HCID 66779757HCID 66779757, 화합물수율 96.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-[5-Bromo-1-(toluene-4-sulfonyl)-1H-pyrrolo[2,3-b]pyridin-3-yl]-benzylamine (Intermediate CB, 45 mg, 0.1 mmol) was combined with triethylamine (45 μl, 0.3 mmol) and acetic anhydride (11 μl, 0.11 mmol) in anh. DCM (2 ml). The mixture was stirred for 2 hrs, EtOAc, was added and washed with 0.5 N HCl, saturated NaHCO3, water and brine. Evaporation yielded the title compound (48 mg, 96%). MS ESI (m/z): 498.1/500.1 (M+1)+, calc. 497/499.

후처리

  1. washwashed with 0.5 N HCl, saturated NaHCO3, water and brine
  2. customEvaporation

출처 및 근거

ORD 기록
ord-3b8d39fa73e646d3b5e852cdee7b941f
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181247B2

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