Diethyl Ether → [4-(Benzyloxy)benzyl](triphenyl)phosphonium chloride

HRID 1431912

反応式

HRID 1431912 の反応式
[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH2:13][Cl:14])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:17]1([P:23]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.CCOCC>C1(C)C=CC=CC=1>[Cl-:14].[CH2:1]([O:8][C:9]1[CH:16]=[CH:15][C:12]([CH2:13][P+:23]([C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 11776TriphenylphosphineHCID 700424-Benzyloxybenzyl chloride

生成物 1

HCID 383834[4-(Benzyloxy)benzyl](triphenyl)phosphonium chloride

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

4-Benzyloxybenzyl chloride (1 g, 0.0043 moles) and triphenyl phosphine (1.127 g, 1 equivalent) in anhydrous toluene (20 mL) were refluxed under nitrogen for ˜8-10 hours. A white precipitate appeared in the reaction mixture. The reaction mixture was then cooled to room temperature and ether (100 mL) was added. The precipitated phosphonium salt was collected by filtration, rinsed with ether and air dried. Yield=0.55 g (25%). MALDI-TOF MS 459.51 obs. (459.54 calc.).

後処理

  1. filtrationThe precipitated phosphonium salt was collected by filtration
  2. washrinsed with ether and air
  3. customdried

出典と根拠

ORDレコード
ord-e565d9f02d4240609cdd5106b7ef50da
出典データセット
uspto-grants-2009_11
特許番号
US07611909B1

関連ノート

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