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

HRID 277345

반응식

HRID 277345 반응식
[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

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 11776TriphenylphosphineHCID 700424-Benzyloxybenzyl chloride

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.).

후처리

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

출처 및 근거

ORD 기록
ord-5fec410a09354eb1a80b0b1332618c8c
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06355803B1

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