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

HRID 1685536ノート

反応式

HRID 1685536 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8ce18b69026c4a3ebebdc9db287193f0
出典データセット
uspto-grants-2012_04
特許番号
US08148412B2

反応ノート

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