Iodoethane → 3,5-Dichlorophenyl ethyl sulfide

HRID 75230

反応式

HRID 75230 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([SH:9])[CH:5]=[C:6]([Cl:8])[CH:7]=1.I[CH2:11][CH3:12].C(=O)([O-])[O-].[K+].[K+].C(Cl)Cl>O>[CH2:11]([S:9][C:4]1[CH:3]=[C:2]([Cl:1])[CH:7]=[C:6]([Cl:8])[CH:5]=1)[CH3:12]

参加物

6

反応物 4

HCID 6340IodoethaneHCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 27360963,5-Dichlorobenzenethiol

生成物 1

HCID 597520583,5-Dichlorophenyl ethyl sulfide収率 97.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 3,5-dichlorobenzenethiol (1.50 g, 8.4 mmol), iodoethane (1.34 mL, 16.8 mmol), potassium carbonate (1.74 g, 12.6 mmol) and methylene chloride (10 mL) was stirred at 25° C. for 30 minutes. The reaction was diluted with water and extracted with ethyl acetate three times, dried over sodium sulfate, filtered and concentrated. The residue was purified by chromatography on silica gel to give the desired product (1.69 g, 97%). LC/MS: 207 (M+H)+.

後処理

  1. extractionextracted with ethyl acetate three times
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-9402da52b7b946efb3caf5900f1f5e5b
出典データセット
uspto-grants-2014_09
特許番号
US08835423B2

関連ノート

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