Acetic Anhydride → HCID 66779757、化合物

HRID 85056ノート

反応式

HRID 85056 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 66779757HCID 66779757、化合物収率 96.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-3996b54ae1f547249b0f2ab9372287bf
出典データセット
uspto-grants-2014_09
特許番号
US08846909B2

反応ノート

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