Triethylamine → p-BROMOPHENYL 1-(p-CHLOROPHENYLSULFONYL)VINYL SULFIDE

HRID 1156385ノート

反応式

HRID 1156385 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH:9]([S:12]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)(=[O:14])=[O:13])[CH2:10]Cl)=[CH:4][CH:3]=1.C(N(CC)CC)C>O1CCCC1.C(OCC)C>[Cl:21][C:18]1[CH:17]=[CH:16][C:15]([S:12]([C:9]([S:8][C:5]2[CH:4]=[CH:3][C:2]([Br:1])=[CH:7][CH:6]=2)=[CH2:10])(=[O:14])=[O:13])=[CH:20][CH:19]=1

参加物

5

反応物 2

HCID 8471TriethylamineHCID 130448002-CHLORO-1-(p-CHLOROPHENYLSULFONYL)ETHYL p-BROMOPHENYL SULFIDE

生成物 1

HCID 13044811p-BROMOPHENYL 1-(p-CHLOROPHENYLSULFONYL)VINYL SULFIDE収率 40.7%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Thirty-five grams (82 mmoles) of 2-chloro-1-(p-chlorophenylsulfonyl)ethyl p-bromophenyl sulfide was dissolved in 100 ml of tetrahydrofuran and treated with 12 ml (86 mmoles) of triethylamine. The mixture was diluted with 100 ml of diethyl ether and allowed to stand for 15 minutes. The precipitated triethylamine hydrochloride was separated by filtration. Evaporation of solvent from the filtrate gave 35 g of crude solid m.p. 45°-95°. Recrystallization from 100 ml of ethyl acetate-pentane (45:55) gave 13 g of pure product, m.p. 97°-99°.

後処理

  1. customThe precipitated triethylamine hydrochloride was separated by filtration
  2. customEvaporation of solvent from the filtrate
  3. customgave 35 g of crude solid m.p. 45°-95°
  4. customRecrystallization from 100 ml of ethyl acetate-pentane (45:55)

出典と根拠

ORDレコード
ord-eb4557c5d75a4e4ab7e7818c24cc9fc8
出典データセット
uspto-grants-1982_06
特許番号
US04335142

反応ノート

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