Diethylcarbamoyl chloride → 1-chloro-1-(4-chlorophenyl)-2-(N,N-diethylcarbamoyloxy)-2-methoxyiminoethane

HRID 1578605노트

반응식

HRID 1578605 반응식
[CH3:1][O:2][NH:3][C:4](=[O:14])[CH:5]([C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1)[Cl:6].C(N(CC)CC)C.[CH2:22]([N:24]([CH2:28][CH3:29])[C:25](Cl)=[O:26])[CH3:23]>C1C=CC=CC=1>[Cl:6][CH:5]([C:7]1[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][CH:8]=1)[C:4]([O:14][C:25](=[O:26])[N:24]([CH2:28][CH3:29])[CH2:22][CH3:23])=[N:3][O:2][CH3:1]

참가 물질

5

반응물 3

HCID 6916Diethylcarbamoyl chlorideHCID 8471TriethylamineHCID 152693932-chloro-2-(4-chlorophenyl)-N-methoxyacetamide

생성물 1

HCID 539660661-chloro-1-(4-chlorophenyl)-2-(N,N-diethylcarbamoyloxy)-2-methoxyiminoethane

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

N-Methoxy-α-(4-chlorophenyl)-α-chloroacetamide (23.3 grams; 0.1 mole), benzene (100 ml), and triethylamine (12 grams; 0.12 mole) are charged into a glass reaction flask equipped with a mechanical stirrer, thermometer and reflux condenser. N,N-Diethylcarbamoyl chloride (13.5 grams; 0.1 mole) dissolved in benzene (25 ml) is incrementally added to the reaction mixture, with stirring, at room temperature. After the addition is completed the reaction mixture is heated at reflux for a period of about 4 hours. After this time the reaction mixture is distilled to remove benzene and unreacted starting material thereby yielding the desired product 1-chloro-1-(4-chlorophenyl)-2-(N,N-diethylcarbamoyloxy)-2-methoxyiminoethane.

후처리

  1. customequipped with a mechanical stirrer
  2. temperaturethermometer and reflux condenser
  3. additionis incrementally added to the reaction mixture
  4. additionAfter the addition
  5. temperatureis heated
  6. temperatureat reflux for a period of about 4 hours
  7. distillationAfter this time the reaction mixture is distilled
  8. customto remove benzene

출처 및 근거

ORD 기록
ord-f0569bc5dbf94735b9fb04b3256c644e
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03937824

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