Triethylamine → 1-Methyl-1H-pyrazole-4-sulfonic acid (2,2-dimethoxy-ethyl)-methyl-amide

HRID 553499ノート

反応式

HRID 553499 の反応式
[CH3:1][O:2][CH:3]([O:7][CH3:8])[CH2:4][NH:5][CH3:6].C(N(CC)CC)C.[CH3:16][N:17]1[CH:21]=[C:20]([S:22](Cl)(=[O:24])=[O:23])[CH:19]=[N:18]1>C(Cl)Cl>[CH3:1][O:2][CH:3]([O:7][CH3:8])[CH2:4][N:5]([CH3:6])[S:22]([C:20]1[CH:19]=[N:18][N:17]([CH3:16])[CH:21]=1)(=[O:24])=[O:23]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 85032,2-DimethoxyethylmethylamineHCID 170247301-methyl-1H-pyrazole-4-sulfonyl chloride

生成物 1

HCID 673674041-Methyl-1H-pyrazole-4-sulfonic acid (2,2-dimethoxy-ethyl)-methyl-amide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Cool a solution of methylaminoacetaldehyde dimethyl acetal (22.5 mL, 0.18 mol) and triethylamine (26.5 mL, 0.19 mol) to 0° C. in CH2Cl2, then add dropwise a solution of 1-methyl-1H-pyrazole-4-sulfonyl chloride (30 g, 0.17 mol). Stir the reaction mixture at room temperature overnight, dilute with CH2Cl2 (500 mL), and wash with water. Dry the combined organics over Na2SO4, filter and concentrate. The resulting oil is placed under high vacuum and within two hours a resulting off white solid is formed, which is used without further purification (38.22 g, 87%).

後処理

  1. washwash with water
  2. dry with materialDry the combined organics over Na2SO4
  3. filtrationfilter
  4. concentrationconcentrate
  5. waitThe resulting oil is placed under high vacuum and within two hours
  6. customa resulting off white solid is formed
  7. customwhich is used without further purification (38.22 g, 87%)

出典と根拠

ORDレコード
ord-d2543f19f53948808fec9e1c51aa7f39
出典データセット
uspto-grants-2011_11
特許番号
US08048884B2

反応ノート

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