Acetic Anhydride → N-[4-Methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-yl]-acetamide

HRID 1951193노트

반응식

HRID 1951193 반응식
[C:1](OC(=O)C)(=[O:3])[CH3:2].[CH3:8][C:9]1[N:10]=[C:11]([NH2:26])[S:12][C:13]=1[C:14]1[CH:19]=[CH:18][N:17]=[C:16]([N:20]2[CH2:25][CH2:24][O:23][CH2:22][CH2:21]2)[N:15]=1>>[CH3:8][C:9]1[N:10]=[C:11]([NH:26][C:1](=[O:3])[CH3:2])[S:12][C:13]=1[C:14]1[CH:19]=[CH:18][N:17]=[C:16]([N:20]2[CH2:25][CH2:24][O:23][CH2:22][CH2:21]2)[N:15]=1

참가 물질

3

반응물 2

HCID 7918Acetic AnhydrideHCID 866103364-Methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-ylamine

생성물 1

HCID 86610334N-[4-Methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-yl]-acetamide

반응 조건

온도
60 °C

실험 절차

Acetic anhydride (3 ml) is added to 4-methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-ylamine (25d)(0.045 g, 0.162 mmol) and the reaction mixture is heated to 60° C. for 1 hour. The solvent is removed in vacuo and the crude residue is dissolved in ethyl acetate (50 ml) and water (50 ml) The layers are separated and the organic layer is washed with sodium carbonate solution, brine, dried over MgSO4 and concentrated in vacuo to yield a brown oil. The crude residue is purified by chromatography on silica eluting with ethyl acetate-hexane (3:2) to afford the titled compound.

후처리

  1. customThe solvent is removed in vacuo
  2. dissolutionthe crude residue is dissolved in ethyl acetate (50 ml)
  3. customwater (50 ml) The layers are separated
  4. washthe organic layer is washed with sodium carbonate solution, brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. customto yield a brown oil
  8. customThe crude residue is purified by chromatography on silica eluting with ethyl acetate-hexane (3:2)

출처 및 근거

ORD 기록
ord-18f85d6c98c6474b85b59aaf684df4a0
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404684B2

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