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

HRID 507695노트

반응식

HRID 507695 반응식
[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

참가 물질

5

반응물 1

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

생성물 1

HCID 110628127-Chloro-1-benzothiophene

시약·촉매·용매 3

HCID 23978Copper촉매HCID 313Hydrochloric Acid용매HCID 7047Quinoline용매

반응 조건

온도
190 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aa344c28fe954e759cd1d0608982e5e6
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786132B2

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