Dichloromethane → HCID 66968119、化合物

HRID 70740

反応式

HRID 70740 の反応式
[C:1]1([C:7]2[CH2:12][CH2:11][CH2:10][CH2:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[S:13]1[CH:17]=[CH:16][CH:15]=[CH:14]1.ClCCl>Br.C(O)(=O)C>[C:1]1([C:7]2([C:14]3[S:13][CH:17]=[CH:16][CH:15]=3)[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

6

反応物 3

HCID 6344DichloromethaneHCID 8030ThiopheneHCID 130431-Phenylcyclohexene

生成物 1

HCID 66968119HCID 66968119、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 260Hydrogen Bromide溶媒

実験手順

Phenyl cyclohexene (50 mg) and thiophene (100 mg) were dissolved in 33% HBr in acetic acid (0.5 mL). The mixture was stirred at room temperature over night. Tlc indicated full conversion of the starting material. Dichloromethane (10 mL) was added. The organic phase was washed with saturated NaHCO3 (3×10 mL), dried Na2SO4 and concentrated in vacuo. The desired product was afforded after flash chromatography (eluent: dichloromethane). Yield: 39 mg. LC/MS purity (UV/MS): 100/90%, Rt 6.22 min. M+1: 243

後処理

  1. washThe organic phase was washed with saturated NaHCO3 (3×10 mL), dried Na2SO4
  2. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-7c2b84a7b779425e99164e43cf496820
出典データセット
uspto-grants-2014_09
特許番号
US08822548B2

関連ノート

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