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

HRID 54276

반응식

HRID 54276 반응식
[C:1]1([P:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Br:20][CH2:21][Br:22]>C1(C)C=CC=CC=1>[Br-:20].[Br:22][CH2:21][P+:7]([C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 3024DibromomethaneHCID 11776Triphenylphosphine

생성물 1

HCID 2733422Phosphonium, (bromomethyl)triphenyl-, bromide (1:1)수율 78.3%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Under a nitrogen atmosphere, a stirred solution of 215.0 grams (0.82 mole) of triphenylphosphine and 115 mL (1.64 moles) of dibromomethane in 600 mL of toluene was heated at reflux for about eight hours. After this time a solid was collected by filtration. The filtrate was again heated to reflux where it stirred for an additional eight hours. The mixture was cooled and additional solid was collected by filtration. The two solids were combined, yielding about 280 grams of bromomethyl triphenylphosphonium bromide.

후처리

  1. temperatureat reflux for about eight hours
  2. filtrationAfter this time a solid was collected by filtration
  3. temperatureThe filtrate was again heated
  4. temperatureto reflux where it
  5. temperatureThe mixture was cooled
  6. filtrationadditional solid was collected by filtration

출처 및 근거

ORD 기록
ord-4c6ba2453a834a448a547250555fd250
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05622954

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