7-Chloro-1-benzothiophene-2-carboxylic acid → 7-Chloro-1-benzothiophene

HRID 507695ノート

反応式

HRID 507695 の反応式
[Cl:1][C:2]1[C:7]2[S:8][C:9](C(O)=O)=[CH:10][C:6]=2[CH:5]=[CH:4][CH:3]=1>N1C2C(=CC=CC=2)C=CC=1.Cl.[Cu]>[Cl:1][C:2]1[C:7]2[S:8][CH:9]=[CH:10][C:6]=2[CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 1

HCID 101982427-Chloro-1-benzothiophene-2-carboxylic acid

生成物 1

HCID 110628127-Chloro-1-benzothiophene

試薬・触媒・溶媒 3

HCID 23978Copper触媒HCID 313Hydrochloric Acid溶媒HCID 7047Quinoline溶媒

反応条件

温度
190 °C

実験手順

7-Chlorobenzo[b]thiophene-2-carboxylic acid (2.5 g, 11.8 mmol) was suspended in quinoline (20 mL) and treated with copper (0.779 g, 13 mmol). The mixture was heated to 190° C. After 1.5 h, the mixture was allowed to cool down to room temperature and diluted with 200 mL of 2 N HCl. The mixture was extracted three times with ethyl acetate. All the organic layers were combined and washed with 1 N HCl, water and brine, then dried with sodium sulfate. Purification was achieved by flash chromatography using 10 to 20% ethyl acetate in hexanes. Yield=1.8 g.

後処理

  1. temperatureto cool down to room temperature
  2. extractionThe mixture was extracted three times with ethyl acetate
  3. washwashed with 1 N HCl, water and brine
  4. dry with materialdried with sodium sulfate
  5. customPurification

出典と根拠

ORDレコード
ord-aa344c28fe954e759cd1d0608982e5e6
出典データセット
uspto-grants-2010_08
特許番号
US07786132B2

反応ノート

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