1,2-Bis(chloromethyl)benzene → 2-(Chloromethyl)benzyltriethylphosphonium chloride

HRID 375018

반응식

HRID 375018 반응식
[Cl:1][CH2:2][C:3]1[C:4]([CH2:9][Cl:10])=[CH:5][CH:6]=[CH:7][CH:8]=1.[CH2:11]([P:13]([CH2:16][CH3:17])[CH2:14][CH3:15])[CH3:12].[Cl-].C([PH+](CC)CC)C>C1(C)C=CC=CC=1>[Cl-:1].[Cl:10][CH2:9][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[CH2:2][P+:13]([CH2:16][CH3:17])([CH2:14][CH3:15])[CH2:11][CH3:12]

참가 물질

5

반응물 3

HCID 119191,2-Bis(chloromethyl)benzeneHCID 27365TriethylphosphineHCID 19032181Triethylphosphonium chloride salt

생성물 1

HCID 190321702-(Chloromethyl)benzyltriethylphosphonium chloride

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a mixture of α,α'-dichloro-o-xylene (15.0 g, 86.0 mmol) in toluene (200 ml) was added triethylphosphine (6.3 ml, 43.0 mmol) under argon gas. The reaction mixture was stirred for several days at room temperature under argon after which time the triethylphosphonium chloride salt had crystallized out of solution. The crystals were filtered and washed with toluene (3×50 mL) and pentane (3×50 mL) and dried: 1H NMR (CDCl3) δ1.15-1.26 (dt, 9), 2.58-2.69 (m, 6H), 4.39-4.44 (d, 2H), 4.87 (s, 2H) , 7.31-7.34 (dd, 2H) , 7.43-7.46 (dd, 1H), 7.50-7.54 (m, 1H).

후처리

  1. customhad crystallized out of solution
  2. filtrationThe crystals were filtered
  3. washwashed with toluene (3×50 mL) and pentane (3×50 mL)
  4. customdried

출처 및 근거

ORD 기록
ord-10ae76f6ec0f4443944228377f5b406d
출처 데이터셋
uspto-grants-1996_01
특허 번호
US05484556

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