Thionyl Chloride → HCID 9998156、化合物

HRID 1354815ノート

反応式

HRID 1354815 の反応式
[CH2:1]([O:8][C:9]1[CH:17]=[C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:15]=[CH:14][C:10]=1[C:11](O)=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:28])=O>CN(C=O)C>[CH2:1]([O:8][C:9]1[CH:17]=[C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:15]=[CH:14][C:10]=1[C:11]([Cl:28])=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 9840634HCID 9840634、化合物

生成物 1

HCID 9998156HCID 9998156、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide触媒

実験手順

Compound 37 (1 g, 3 mmol) was mixed with thionyl chloride (7.2 g, 60 mmol) and 3 drops of DMF. The reaction mixture was refluxed for 3 h under nitrogen. After cooling down to room temperature, thionyl chloride was removed under reduced pressure. Toluene (5 mL) was then added, and the mixture was dried under reduced pressure again. This process was repeated twice to ensure all the excess of thionyl chloride was removed. The compound 38 was further dried under high vacuum for half an hour and was used directly in the next step without purification.

後処理

  1. temperatureThe reaction mixture was refluxed for 3 h under nitrogen
  2. customthionyl chloride was removed under reduced pressure
  3. additionToluene (5 mL) was then added
  4. customthe mixture was dried under reduced pressure again
  5. customwas removed
  6. dry with materialThe compound 38 was further dried under high vacuum for half an hour
  7. customwas used directly in the next step without purification

出典と根拠

ORDレコード
ord-5495d8a47fb143efa8747edd59817654
出典データセット
uspto-grants-2007_05
特許番号
US07223759B2

反応ノート

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