2-Pentylthiophene → 2-bromo-5-pentylThiophene
반응식
[CH2:1]([C:6]1[S:7][CH:8]=[CH:9][CH:10]=1)[CH2:2][CH2:3][CH2:4][CH3:5].[Br:11]N1C(=O)CCC1=O.C(O)(=O)C.C(Cl)(Cl)Cl>O>[Br:11][C:8]1[S:7][C:6]([CH2:1][CH2:2][CH2:3][CH2:4][CH3:5])=[CH:10][CH:9]=1참가 물질
5
실험 절차
A solution of 2-pentylthiophene, (25.2 g) N-bromosuccinimide (25.5 g) and a 1:1 chloroform acetic acid mixture (100 cm3) was heated under reflux for 1 h. Water (10 cm3) was added and the resultant solution stirred for 10 min under an atmosphere of nitrogen. The organic layer was separated off and the aqueous layer extracted with diethyl ether (2×50 cm3). The combined organic layers were washed with brine (2×100 cm3), dried (MgSO4), filtered and then evaporated down. The residue was purified by distillation (Bp 132-134° C. at 15-20 mm Hg.) to yield 32.6 g of 2-bromo-5-pentylthiophene.
후처리
- temperatureunder reflux for 1 h
- customThe organic layer was separated off
- extractionthe aqueous layer extracted with diethyl ether (2×50 cm3)
- washThe combined organic layers were washed with brine (2×100 cm3)
- dry with materialdried (MgSO4)
- filtrationfiltered
- customevaporated down
- distillationThe residue was purified by distillation (Bp 132-134° C. at 15-20 mm Hg.)
출처 및 근거
- ORD 기록
- ord-76bad079f71b44409d06f5ec6a1ec022
- 출처 데이터셋
- uspto-grants-2004_02
- 특허 번호
- US06696110B1
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