Potassium Hydroxide → HCID 19738531、化合物

HRID 1460769ノート

反応式

HRID 1460769 の反応式
[CH3:1][O:2][CH:3]([O:11][CH3:12])[CH2:4][NH:5][C:6](=[O:10])[O:7][CH2:8][CH3:9].[OH-].[K+].[Cl:15][C:16](=[CH2:19])[CH2:17]I>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C.C1(C)C=CC=CC=1>[Cl:15][C:16](=[CH2:17])[CH2:19][N:5]([CH2:4][CH:3]([O:2][CH3:1])[O:11][CH3:12])[C:6](=[O:10])[O:7][CH2:8][CH3:9]

参加物

6

反応物 3

HCID 14797Potassium Hydroxide2 回HCID 10921057Ethyl 2,2-dimethoxyethylcarbamateHCID 109435662-Chloro-3-iodoprop-1-ene2 回

生成物 1

HCID 19738531HCID 19738531、化合物

試薬・触媒・溶媒 2

HCID 66133Benzyl triethylammonium chloride触媒2 回HCID 1140Toluene溶媒

実験手順

115 g (0.65 mol) of ethyl N-(2,2-dimethoxyethyl) -carbamate, 130 g of powdered potassium hydroxide and 2 g of triethylbenzylammonium chloride are initially introduced into 650 ml of toluene and 142 g (0.7 mol) of 2-chloroallyl iodide are added dropwise at room temperature. After stirring overnight, a gas chromatogram showed incomplete conversion, hence 65 g of powdered potassium hydroxide and 1 g of triethylbenzylammonium chloride were added again and a further 71 g (0.35 mol) of 2-chloroallyl iodide were added dropwise. After stirring overnight at room temperature, the salts were filtered off with suction, the filtrate was washed with saturated sodium chloride solution, dried over magnesium sulphate and concentrated, and the residue was distilled.

後処理

  1. additionare added dropwise at room temperature
  2. additionwere added again
  3. stirringAfter stirring overnight at room temperature
  4. filtrationthe salts were filtered off with suction
  5. washthe filtrate was washed with saturated sodium chloride solution
  6. dry with materialdried over magnesium sulphate
  7. concentrationconcentrated
  8. distillationthe residue was distilled

出典と根拠

ORDレコード
ord-d644888567ac42bcaee13a3a4e19dfe0
出典データセット
uspto-grants-1991_12
特許番号
US05071999

反応ノート

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