Methanol → 4-Methyl-5-(4-methyl-piperazine-1-sulfonyl)-thiazol-2-ylamine

HRID 1685536노트

반응식

HRID 1685536 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([S:8]([C:11]2[S:15][C:14]([NH:16]C(=O)C)=[N:13][CH:12]=2)(=[O:10])=[O:9])[CH2:4][CH2:3]1.[CH3:20]O>Cl>[CH3:20][C:12]1[N:13]=[C:14]([NH2:16])[S:15][C:11]=1[S:8]([N:5]1[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1)(=[O:10])=[O:9]

참가 물질

4

반응물 2

HCID 887MethanolHCID 42560673Acetamide, N-[5-[(4-methyl-1-piperazinyl)sulfonyl]-2-thiazolyl]-

생성물 1

HCID 639461724-Methyl-5-(4-methyl-piperazine-1-sulfonyl)-thiazol-2-ylamine

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of N-[5-(4-methylpiperazine-1-sulfonyl)-thiazol-2-yl]-acetamide (1 g, 3.1 mmol) in methanol (5 mL) and 6 N hydrochloric acid (5 mL) was heated in a microwave oven (4×5 min at 80° C.). The reaction mixture was partly evaporated to remove most of the methanol, and the residue was washed with DCM (10 mL). The water phase was isolated, and the pH adjusted to 8-9. Extraction with DCM (3×25 mL), drying over anhydrous magnesium sulphate, and evaporation in vacuo gave white crystals of 4-methyl-5-(4-methyl-piperazine-1-sulfonyl)-thiazol-2-ylamine. Yield: 0.53 g (61%). 1H-NMR (CDCl3): δ 5.46 (m, 2H); 3.18 (m, 4H); 2.51 (m, 4H); 2.45 (s, 3H); 2.31 (s, 3H).

후처리

  1. customThe reaction mixture was partly evaporated
  2. customto remove most of the methanol
  3. washthe residue was washed with DCM (10 mL)
  4. customThe water phase was isolated
  5. extractionExtraction with DCM (3×25 mL)
  6. dry with materialdrying over anhydrous magnesium sulphate, and evaporation in vacuo

출처 및 근거

ORD 기록
ord-8ce18b69026c4a3ebebdc9db287193f0
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148412B2

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