Methanol → Phosphonium, (bromomethyl)triphenyl-, bromide (1:1)

HRID 399111

反応式

HRID 399111 の反応式
[Br-:1].[C:2]1([PH+:8]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P(Br)(Br)[Br:22].[CH3:25]O>C1C=CC=CC=1>[Br-:22].[Br:1][CH2:25][P+:8]([C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

参加物

5

反応物 3

HCID 887MethanolHCID 24614Phosphorus tribromideHCID 517696Phosphine, triphenyl-, hydrobromide

生成物 1

HCID 2733422Phosphonium, (bromomethyl)triphenyl-, bromide (1:1)

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
25 °C

実験手順

A mixture of hydroxymethyl)triphenylphosphonium bromide and phosphorus tribromide in benzene is heated at reflux for 23 h with stirring. After this time the solution is dark orange and an orange solid is present. The mixture is cooled to 25° C. and methanol is added. The solvent was removed at reduced pressure and the residue treated with water to extract the phosphonium salt. The aqueous extracts were saturated with solid potassium bromide and extracted with chloroform. The phosphonium salts are crystallized from hot chloroform by addition of ethyl acetate.

後処理

  1. temperatureis heated
  2. temperatureat reflux for 23 h
  3. customThe solvent was removed at reduced pressure
  4. additionthe residue treated with water
  5. extractionto extract the phosphonium salt
  6. extractionextracted with chloroform
  7. customThe phosphonium salts are crystallized from hot chloroform by addition of ethyl acetate

出典と根拠

ORDレコード
ord-7237fbfbfe244ea4b5590452eb3af00b
出典データセット
uspto-grants-1998_10
特許番号
US05817776

関連ノート

読み込み中…