Benzene → Phenoxyacetylmethyltriphenylphosphonium Chloride

HRID 893893ノート

反応式

HRID 893893 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-8ce62c1cdc384a17937a097dcf9d27d8
出典データセット
uspto-grants-1981_08
特許番号
US04282149

反応ノート

読み込み中…