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

HRID 54276

反応式

HRID 54276 の反応式
[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

参加物

4

反応物 2

HCID 3024DibromomethaneHCID 11776Triphenylphosphine

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4c6ba2453a834a448a547250555fd250
出典データセット
uspto-grants-1997_04
特許番号
US05622954

関連ノート

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