Hydrochloric Acid → 4-Methoxy-3-(2-phenylethyl)benzo[b]thiophene

HRID 230884노트

반응식

HRID 230884 반응식
C([C:4]1[S:8][C:7]2[CH:9]=[CH:10][CH:11]=[C:12]([O:13][CH3:14])[C:6]=2[C:5]=1[CH2:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)(O)=O.Cl>N1C2C(=CC=CC=2)C=CC=1.[Cu]>[CH3:14][O:13][C:12]1[C:6]2[C:5]([CH2:15][CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[CH:4][S:8][C:7]=2[CH:9]=[CH:10][CH:11]=1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 231035202-Carboxy-4-methoxy-3-(2-phenylethyl)benzo[b]thiophene

생성물 1

HCID 231035114-Methoxy-3-(2-phenylethyl)benzo[b]thiophene수율 89.6%

시약·촉매·용매 2

HCID 23978Copper촉매HCID 7047Quinoline용매

실험 절차

A suspension of 2-carboxy-4-methoxy-3-(2-phenylethyl)benzo[b]thiophene (1 g) and a catalytic amount of copper powder in quinoline (15 mL) was stirred at 200° C. for 2 hours. The reaction mixture was cooled to room temperature and poured into 1 mol/L hydrochloric acid, and the resulting mixture was extracted with ethyl acetate. The extract was washed with 1 mol/L hydrochloric acid and water, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=5/1) to give the title compound (0.77 g).

후처리

  1. extractionthe resulting mixture was extracted with ethyl acetate
  2. washThe extract was washed with 1 mol/L hydrochloric acid and water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=5/1)

출처 및 근거

ORD 기록
ord-50415b8d3c7d4c0d81ff32d21763ee6f
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566699B2

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