Hydrochloric Acid → HCID 19091987、化合物

HRID 487526ノート

反応式

HRID 487526 の反応式
[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]

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 702EthanolHCID 31374DimethylacetamideHCID 3045879Acetic acid, (p-aminobenzoyl)-, ethyl ester (6CI,7CI)HCID 125892012-Chlorosulfonylbutyl chloride

生成物 1

HCID 19091987HCID 19091987、化合物

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dddf2d00a6de4b4c9a4eaf8c36c60901
出典データセット
uspto-grants-1994_03
特許番号
US05296344

反応ノート

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