Hydrochloric Acid → HCID 19091987, 화합물

HRID 487526

반응식

HRID 487526 반응식
[CH2:1]([OH:3])[CH3:2].Cl[S:5]([CH:8]([CH2:11][CH3:12])[CH2:9]Cl)(=[O:7])=[O:6].[NH2:13][C:14]1[CH:27]=[CH:26][C:17]([C:18]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:19])=[CH:16][CH:15]=1.Cl.CN(C)C(=[O:33])C>N1C=CC=CC=1.O1CCCC1>[CH2:1]([O:3][C:9]([CH:8]([S:5]([NH:13][C:14]1[CH:15]=[CH:16][C:17]([C:18]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:19])=[CH:26][CH:27]=1)(=[O:7])=[O:6])[CH2:11][CH3:12])=[O:33])[CH3:2]

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 702EthanolHCID 31374DimethylacetamideHCID 3045879Acetic acid, (p-aminobenzoyl)-, ethyl ester (6CI,7CI)HCID 12589201HCID 12589201, 화합물

생성물 1

HCID 19091987HCID 19091987, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 8028Tetrahydrofuran용매2회

실험 절차

Ethanol (3.6 g) and tetrahydrofuran (10 ml) were dropwise added to a solution of 2-chlorosulfonylbutyl chloride (14.4 g) and tetrahydrofuran (21 ml) while cooling with ice. After stirring at room temperature for 1 hour, ethyl p-aminobenzoylacetate (13.3 g), N,N-dimethylacetamide (33 ml) and pyridine (12.2 g) were added thereto, and the mixture was heated for refluxing for 30 minutes. 0.5 N hydrochloric acid (30 ml) was added to the reaction solution, and the mixture was extracted with ethyl acetate (120 ml). The extracted solution was washed with a sodium chloride aqueous solution (120 ml), then dried over magnesium sulfate, and concentrated. An oily product, ethyl p-(1-ethoxycarbonylpropanesulfonamido)benzoylacetate was quantitatively obtained.

후처리

  1. temperaturewhile cooling with ice
  2. temperaturethe mixture was heated
  3. temperaturefor refluxing for 30 minutes
  4. extractionthe mixture was extracted with ethyl acetate (120 ml)
  5. washThe extracted solution was washed with a sodium chloride aqueous solution (120 ml)
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-dddf2d00a6de4b4c9a4eaf8c36c60901
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05296344

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