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Acetyl chloride → N-Allyl-N-(2,2-dimethoxyethyl)acetamide

HRID 1646104
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HRID 1646104 반응식
[CH2:1]([NH:4][CH2:5][CH:6]([O:9][CH3:10])[O:7][CH3:8])[CH:2]=[CH2:3].[OH-].[Na+].[C:13](Cl)(=[O:15])[CH3:14]>C1(C)C=CC=CC=1>[CH2:1]([N:4]([CH2:5][CH:6]([O:9][CH3:10])[O:7][CH3:8])[C:13](=[O:15])[CH3:14])[CH:2]=[CH2:3]
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참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 14798Sodium HydroxideHCID 13334742N-(2,2-Dimethoxyethyl)prop-2-en-1-amine

생성물 1

HCID 45120254N-Allyl-N-(2,2-dimethoxyethyl)acetamide수율 80%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
5 °C

실험 절차

N-allyl-N-dimethoxyethyl amine (30% aqueous, 48.3 grams, 0.10 mole) was added to a glass reaction vessel fitted with a mechanical agitator. The agitator was started and sodium hydroxide (4.44 grams, 0.11 mole) was dissolved in the aqueous amine. Toluene (50 grams) was added and the mixture cooled to 0° to 5° C. Acetyl chloride (8.24 grams, 0.105 mole) was added over 10 minutes while maintaining the temperature below 5° C. The reaction mixture was stirred for 30 minutes at 5° C., agitation was stopped, and the mixture allowed to phase separate. The aqueous layer was discarded. Toluene was removed from the organic layer by rotary evaporation and 14.8 grams (0.08 mole) of N-allyl-N-dimethoxyethyl acetamide was isolated as confirmed by NMR.

후처리

  1. customfitted with a mechanical agitator
  2. temperaturethe mixture cooled to 0° to 5° C
  3. temperaturewhile maintaining the temperature below 5° C
  4. customseparate
  5. customToluene was removed from the organic layer by rotary evaporation

출처 및 근거

ORD 기록
ord-b3fdc222ce294d688cf8c9f09bac0102
출처 데이터셋
uspto-grants-1993_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05177263

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