2-Pentylthiophene → 2-bromo-5-pentylThiophene
反応式
[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]=1参加物
5
実験手順
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.
後処理
- 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.)
出典と根拠
- ORDレコード
- ord-76bad079f71b44409d06f5ec6a1ec022
- 出典データセット
- uspto-grants-2004_02
- 特許番号
- US06696110B1
反応ノート
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