Triethylamine → HCID 22850442, 화합물

HRID 1975300노트

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HRID 1975300 반응식
[CH:1](=[C:5]1/[C:6](=[O:11])[CH2:7][C:8](=[O:10])[NH:9]/1)\[CH:2]([CH3:4])[CH3:3].[C:12](Cl)(=[O:16])[CH2:13][CH2:14][CH3:15].C(N(CC)CC)C>ClCCl>[C:12]([O:11][C:6]1=[CH:7][C:8](=[O:10])[NH:9]/[C:5]/1=[CH:1]\[CH:2]([CH3:4])[CH3:3])(=[O:16])[CH2:13][CH2:14][CH3:15]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 8855Butyryl chlorideHCID 18655319HCID 18655319, 화합물

생성물 1

HCID 22850442HCID 22850442, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
-5 °C

실험 절차

31.8 g of (Z)-5-isobutylidenepyrrolidine-2,4-dione was suspended in 318 ml of dichloromethane and cooled to -5° C. Then first 23.22 g of butyryl chloride was added and then 27.32 g of triethylamine was added. After the addition the mixture was stirred another 10 minutes at 0° C., then diluted with 100 ml of dichloromethane, and washed twice with 100 ml of 5 percent NaHCO3 solution each and twice with 100 ml of 0.4M hydrochloric acid each. The aqueous phases were extracted separately with dichloromethane and the combined organic phases were dried on magnesium sulfate. After the distilling off of the solvent, the crude product (46 g) was recrystallized from hexane. The yield of the title compound was 38.8 g (84 percent of theory). The title compound had a melting point of 111° to 112° C. Other data concerning the title compound was:

후처리

  1. additionAfter the addition the mixture
  2. washwashed twice with 100 ml of 5 percent NaHCO3 solution each and twice with 100 ml of 0.4M hydrochloric acid each
  3. extractionThe aqueous phases were extracted separately with dichloromethane
  4. customthe combined organic phases were dried on magnesium sulfate
  5. customAfter the distilling off of the solvent, the crude product (46 g) was recrystallized from hexane

출처 및 근거

ORD 기록
ord-1a43a081ec044787a43eec255bcd5ab2
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05286650

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