Isopropanol → Benzenemethanaminium, N,N,N-tributyl-2,4-dichloro-, chloride

HRID 1154978노트

반응식

HRID 1154978 반응식
[CH2:1]([N: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][C:15]1[CH:22]=[C:21]([Cl:23])[CH:20]=[CH:19][C:16]=1[CH2:17]Cl.C(O)(C)C>O>[Cl-:14].[CH2:10]([N+:5]([CH2:1][CH2:2][CH2:3][CH3:4])([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:17][C:16]1[CH:19]=[CH:20][C:21]([Cl:23])=[CH:22][C:15]=1[Cl:14])[CH2:11][CH2:12][CH3:13]

참가 물질

5

반응물 3

HCID 3776Isopropanol2회HCID 72122,4-Dichlorobenzyl chlorideHCID 7622Tributylamine2회

생성물 1

HCID 165101Benzenemethanaminium, N,N,N-tributyl-2,4-dichloro-, chloride수율 67%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

One hundred eighty-five and four-tenths parts of tributylamine and 97.8 parts of 2,4-dichlorobenzyl chloride were mixed with 78.5 parts of isopropanol and placed in a reactor equipped with a stirrer, condenser and thermometer. The mixture was heated for 6 hours with stirring at 80° C. after which the isopropanol and excess tributylamine were removed by distillation at 2 mm. and 80° C. 124.2 parts of crude product were obtained. The crude product was dissolved in 300 parts of water, and the water solution was washed with about 50 parts of hexane. The hexane was separated from the water and the water was removed by distillation, giving a recovery from the wash step of 67% tributyl-2,4-dichlorobenzylammonium chloride. Refractive index at 24° C., 1.529; Ionic Cl (Calc.) 9.31%; Cl (found) 9.34% (Volhard).

후처리

  1. customplaced in a reactor
  2. customequipped with a stirrer, condenser
  3. temperatureThe mixture was heated for 6 hours
  4. customwere removed by distillation at 2 mm
  5. custom80° C
  6. custom124.2 parts of crude product were obtained
  7. washthe water solution was washed with about 50 parts of hexane
  8. customThe hexane was separated from the water
  9. customthe water was removed by distillation

출처 및 근거

ORD 기록
ord-c555180d1f9943279e2cdfcac487cbc4
출처 데이터셋
uspto-grants-1981_11
특허 번호
US04299618

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