Benzene → Phenoxyacetylmethyltriphenylphosphonium Chloride

HRID 613978ノート

反応式

HRID 613978 の反応式
[Cl:1][CH2:2][C:3]([CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[O:4].[C:13]1([P:19]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C1C=CC=CC=1>C(Cl)(Cl)Cl>[Cl-:1].[O:6]([CH2:5][C:3]([CH2:2][P+:19]([C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1)([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1)=[O:4])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

5

反応物 3

HCID 241BenzeneHCID 11776TriphenylphosphineHCID 116224561-Chloro-3-phenoxypropan-2-one

生成物 1

HCID 20516787Phenoxyacetylmethyltriphenylphosphonium Chloride

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

1-Chloro-3-phenoxyacetone (13 g, 0.07 mole) dissolved in 20 ml chloroform was mixed with a solution of triphenylphosphine (19.7 g, 1 eq) in 30 ml chloroform at room temperature. The mixture was swirled for 5 minutes and benzene (20 ml) was added. A white crystalline compound appeared when most of the solvents had been evaporated. The product was collected by suction and washed with benzene. Second and third crops were collected by evaporation of the washings. The total yield was 23 g (73%); sublimation without melting at 90°; ir (KBr, cm-1) 3450-3280, 2770, 1720, 1595, 1585, 1485, 1435, 1220, 1110, 1030; nmr (DCCl3, ppm) 8.20-6.80 (m, 22H), 5.30 (br, 2H).

後処理

  1. customhad been evaporated
  2. customThe product was collected by suction
  3. washwashed with benzene
  4. customSecond and third crops were collected by evaporation of the washings

出典と根拠

ORDレコード
ord-ea09d7deb935474b82810f7e4cee1f09
出典データセット
uspto-grants-1979_03
特許番号
US04143046

反応ノート

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