Butyl bromide → Tri-n-octyl-n-butylphosphonium bromide

HRID 258801

반응식

HRID 258801 반응식
[CH2:1]([P:9]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[Br:26][CH2:27][CH2:28][CH2:29][CH3:30]>>[Br-:26].[CH2:18]([P+:9]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])([CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH2:27][CH2:28][CH2:29][CH3:30])[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]

참가 물질

3

반응물 2

HCID 8002Butyl bromideHCID 20851Trioctylphosphine

생성물 1

HCID 22731140Tri-n-octyl-n-butylphosphonium bromide

실험 절차

Tri-n-octyl-n-butylphosphonium bromide is prepared by slowing dripping tri-(n-octyl)phosphine (740 grams) into refluxing 1-bromobutane (500 grams) in a nitrogen atmosphere. Reflux is continued one hour after final addition then the solution is cooled with stirring for about 18 hours, followed by vacuum removal of excess 1-bromobutane at 60° C. This product, 1210 grams from two successive preparations, is added to 880 grams of sodium 3,5-dicarbomethoxybenzenesulfonate in 2500 ml. of water and stirred for at least one hour at 85° C. then the heat is removed and the oil-in-water mixture is stirred for about 18 hours. The oil layer is separated from the water, rinsed with 1000 ml. of water and dried at about 80° C. at a pressure less than 2 torr for 18 hours. This product, an oil, is tri-n-octyl-n-butylphosphonium 3,5-dicarbomethoxybenzenesulfonate with 4.2% phosphorus and 4.7% sulfur by analysis.

후처리

  1. temperatureReflux
  2. additionafter final addition
  3. temperaturethe solution is cooled
  4. customfollowed by vacuum removal of excess 1-bromobutane at 60° C
  5. additionThis product, 1210 grams from two successive preparations, is added to 880 grams of sodium 3,5-dicarbomethoxybenzenesulfonate in 2500 ml
  6. stirringof water and stirred for at least one hour at 85° C.
  7. customthe heat is removed
  8. stirringthe oil-in-water mixture is stirred for about 18 hours
  9. customThe oil layer is separated from the water
  10. washrinsed with 1000 ml
  11. dry with materialof water and dried at about 80° C. at a pressure less than 2 torr for 18 hours

출처 및 근거

ORD 기록
ord-5090c1c29e2b4ff0a00622909c9277ad
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04035346

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