Thionyl Chloride → HCID 19744543、化合物

HRID 2242361ノート

反応式

HRID 2242361 の反応式
S(Cl)([Cl:3])=O.[N:5]1([C:10]2[CH:11]=[C:12]([CH2:16]O)[CH:13]=[CH:14][CH:15]=2)[CH:9]=[CH:8][N:7]=[CH:6]1>CN(C=O)C>[Cl:3][CH2:16][C:12]1[CH:11]=[C:10]([N:5]2[CH:9]=[CH:8][N:7]=[CH:6]2)[CH:15]=[CH:14][CH:13]=1

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 197444983-(1H-Imidazol-1-yl)benzenemethanol

生成物 1

HCID 19744543HCID 19744543、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Thionyl chloride (4.0 ml, 54.0 mmol) was added to a solution of (3-imidazol-1-yl-phenyl)-methanol (3.17 g, 17.0 mmol) in DMF (50 ml) and the reaction stirred at room temperature for 40 h. The solvent was evaporated, the residue diluted with DCM and washed with water, neutralised with aqueous sodium bicarbonate (pH 9-10) and then extracted with DCM (3×). The organic phase was dried over sodium sulfate, filtered and concentrated to give 1-(3-chloromethyl-phenyl)-1H-imidazole as an orange oil (5.3 g, crude contaminated with DMF).

後処理

  1. customThe solvent was evaporated
  2. additionthe residue diluted with DCM
  3. washwashed with water
  4. extractionextracted with DCM (3×)
  5. dry with materialThe organic phase was dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-a6cc3b32698a402ab41ee8462d5c99e9
出典データセット
uspto-grants-2010_03
特許番号
US07671080B2

反応ノート

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