1,2-Bis(chloromethyl)benzene → 2-(Chloromethyl)benzyltri-n-butylphosphonium chloride

HRID 375019노트

반응식

HRID 375019 반응식
[CH2:1]([P:5]([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[Cl:14][CH2:15][C:16]1[C:17]([CH2:22][Cl:23])=[CH:18][CH:19]=[CH:20][CH:21]=1>C1(C)C=CC=CC=1>[Cl-:14].[Cl:23][CH2:22][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[CH2:15][P+:5]([CH2:6][CH2:7][CH2:8][CH3:9])([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:1][CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 119191,2-Bis(chloromethyl)benzeneHCID 13831Tributylphosphine

생성물 1

HCID 676562342-(Chloromethyl)benzyltri-n-butylphosphonium chloride

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

A mixture of tri-n-butylphosphine (18.9 g, 103.8 mmol) in toluene (50 mL) was added dropwise to a mixture of α,α'-dichloro-o-xylene (7.0 g, 34.6 mmol) in toluene (200 mL) under argon gas. The reaction mixture was allowed to stir for several days at room temperature under argon, at which time TLC examination showed completion of reaction. Toluene was removed under reduced pressure to give an oily residue. The above oily residue was washed with toluene/hexane (50/50 (v/v), 4×100 mL), and then dried to give a colorless oil. 1H NMR (CDCl3) δ0.89 (t, 9H), 1.43 (m, 12H), 2.52 (m, 6H), 4.41 (d, 2H), 4.88 (s, 2H), 7.33 (m, 2H), 7.4 5 (m, 1H), 7.52 (m, 1H).

후처리

  1. customcompletion of reaction
  2. customToluene was removed under reduced pressure
  3. customto give an oily residue
  4. washThe above oily residue was washed with toluene/hexane (50/50 (v/v), 4×100 mL)
  5. customdried
  6. customto give a colorless oil

출처 및 근거

ORD 기록
ord-99457bcc819f4162b682d7924cdf7a88
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05484556

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