Acetyl chloride → HCID 178469414、化合物

HRID 2177722ノート

反応式

HRID 2177722 の反応式
C(Cl)(=O)C.[C:5]1([S:11]([CH2:14][C:15]2[C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[C:19]([O:26][CH3:27])[C:18]([C:28]3[N:32](C4CCCCO4)[N:31]=[CH:30][CH:29]=3)=[CH:17][CH:16]=2)(=[O:13])=[O:12])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>CO>[C:5]1([S:11]([CH2:14][C:15]2[C:20]([C:21]([O:23][CH2:24][CH3:25])=[O:22])=[C:19]([O:26][CH3:27])[C:18]([C:28]3[CH:29]=[CH:30][NH:31][N:32]=3)=[CH:17][CH:16]=2)(=[O:13])=[O:12])[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

4

反応物 2

HCID 6367Acetyl chlorideHCID 71268997Ethyl 6-(benzenesulphonylmethyl)-2-methoxy-3-[1-(tetrahydropyran-2-yl)pyrazol-5-yl]benzoate2 回

生成物 1

HCID 178469414HCID 178469414、化合物収率 99.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Acetyl chloride (0.1 ml) was added to methanol (10 ml) cooled in ice and the resultant solution was added to ethyl 6-(benzenesulphonylmethyl)-2-methoxy-3-[1-(tetrahydropyran-2-yl)pyrazol-5-yl]benzoate (Intermediate 47, 0.05 g). The resultant mixture was stirred at room temperature for 1 hour then evaporated to dryness. The residue was treated with sodium bicarbonate (saturated aqueous solution) and extracted with DCM, dried (MgSO4) and filtered. The filtrate was evaporated to dryness to give ethyl 6-(benzenesulphonylmethyl)-2-methoxy-3-(3-pyrazolyl)benzoate (0.041 g) as a gum.

後処理

  1. temperaturecooled in ice
  2. customthen evaporated to dryness
  3. additionThe residue was treated with sodium bicarbonate (saturated aqueous solution)
  4. extractionextracted with DCM
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customThe filtrate was evaporated to dryness

出典と根拠

ORDレコード
ord-9fc4b3acbf2c4ef9b612f2b423b6ba4f
出典データセット
uspto-grants-2015_06
特許番号
US09067905B2

反応ノート

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