Potassium Hydroxide → HCID 19738531, 화합물

HRID 2255701노트

반응식

HRID 2255701 반응식
[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]

참가 물질

6

반응물 3

HCID 14797Potassium Hydroxide2회HCID 10921057Ethyl 2,2-dimethoxyethylcarbamateHCID 109435662-Chloro-3-iodoprop-1-ene2회

생성물 1

HCID 19738531HCID 19738531, 화합물

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride촉매2회HCID 1140Toluene용매

실험 절차

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 2chloroallyl 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.

후처리

  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

출처 및 근거

ORD 기록
ord-e292966163114a43989588e032b9a884
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05241076

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