Benzene, 1,3-bis(chloromethyl)- → 3-(Chloromethyl)benzyltri-n-butylphosphonium chloride

HRID 2399646

반응식

HRID 2399646 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[CH:21]=[CH:20][CH:19]=[C:18]([CH2:22][Cl:23])[CH:17]=1>C1(C)C=CC=CC=1>[Cl-:14].[Cl:23][CH2:22][C:18]1[CH:17]=[C:16]([CH:21]=[CH:20][CH:19]=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 12275Benzene, 1,3-bis(chloromethyl)-HCID 13831Tributylphosphine

생성물 1

HCID 676565363-(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-m-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, after which time the tri-n-butylphosphonium chloride salt had crystallized out of solution and TLC examination showed completion of reaction. The white crystals were filtered and washed several times with toluene and hexanes, and then dried. 1H NMR (CDCl3) δ 0.93 (t, 9H), 1.45 (m, 12H), 2.41 (m, 6H), 4.40 (d, 2H), 4.57 (s, 2H), 7.36 (m, 2H), 7.42 (d, 2H).

후처리

  1. customafter which time the tri-n-butylphosphonium chloride salt had crystallized out of solution and TLC examination
  2. customcompletion of reaction
  3. filtrationThe white crystals were filtered
  4. washwashed several times with toluene and hexanes
  5. customdried

출처 및 근거

ORD 기록
ord-ededb267cad641e9a7f04d2a0d38f761
출처 데이터셋
uspto-grants-1995_09
특허 번호
US05451347

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