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

HRID 6604

反応式

HRID 6604 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 mol) 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-10387fc676524c57a88f49116ff26a5c
出典データセット
uspto-grants-2006_08
特許番号
US07083986B2

関連ノート

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