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

HRID 1154978ノート

反応式

HRID 1154978 の反応式
[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]

参加物

5

反応物 3

HCID 3776Isopropanol2 回HCID 72122,4-Dichlorobenzyl chlorideHCID 7622Tributylamine2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c555180d1f9943279e2cdfcac487cbc4
出典データセット
uspto-grants-1981_11
特許番号
US04299618

反応ノート

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