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

HRID 399111

반응식

HRID 399111 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

반응 조건

온도
25 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7237fbfbfe244ea4b5590452eb3af00b
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05817776

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