Dicyclohexylcarbodiimide → 2-Pyrrolidinone, 1-((4-chlorophenyl)sulfonyl)-

HRID 1762457노트

반응식

HRID 1762457 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][CH2:12][CH2:13][CH2:14][C:15]([OH:17])=O)(=[O:10])=[O:9])=[CH:4][CH:3]=1.C1(N=C=NC2CCCCC2)CCCCC1>O1CCCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]2[CH2:12][CH2:13][CH2:14][C:15]2=[O:17])(=[O:10])=[O:9])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 10868DicyclohexylcarbodiimideHCID 20534824-{[(4-Chlorophenyl)sulfonyl]amino}butanoic acid

생성물 1

HCID 6675352-Pyrrolidinone, 1-((4-chlorophenyl)sulfonyl)-수율 91.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

In 20 ml of tetrahydrofuran was dissolved 2.78 g of N-(4'-chlorobenzenesulfonyl)-4-aminobutyric acid (0.01 mole). To the stirred solution on an ice bath was added 2.06 g of dicyclohexylcarbodiimide (0.01 mole), and the mixture was stirred at 0° C. for 21 hours. The reaction mixture was filtered, and the solid material was washed with anhydrous tetrahydrofuran. The filtrate and the washings were combined, and tetrahydrofuran was removed under reduced pressure. The residue thus obtained was recrystallized from a mixed solvent of chloroform-ether to give 2.37 g of N-(4'-chlorobenzenesulfonyl)-2-pyrrolidone as crystals. Physical properties were identical with those in Synthetic Example 3.

후처리

  1. filtrationThe reaction mixture was filtered
  2. washthe solid material was washed with anhydrous tetrahydrofuran
  3. customtetrahydrofuran was removed under reduced pressure
  4. customThe residue thus obtained
  5. customwas recrystallized from a mixed solvent of chloroform-ether

출처 및 근거

ORD 기록
ord-4e17afe515de4ed6bdec791d6f3984de
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04833156

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