Carbon Tetrachloride → 1-[(2-chloro-1H-pyrrol-1-yl)methyl]-4-propylpyrrolidin-2-one

HRID 1896476노트

반응식

HRID 1896476 반응식
[CH2:1]([CH:4]1[CH2:8][N:7]([CH2:9][N:10]2[CH:14]=[CH:13][CH:12]=[CH:11]2)[C:6](=[O:15])[CH2:5]1)[CH2:2][CH3:3].[Cl:16]N1C(=O)CCC1=O.C(Cl)(Cl)(Cl)Cl>C1COCC1>[Cl:16][C:14]1[N:10]([CH2:9][N:7]2[CH2:8][CH:4]([CH2:1][CH2:2][CH3:3])[CH2:5][C:6]2=[O:15])[CH:11]=[CH:12][CH:13]=1

참가 물질

5

반응물 3

HCID 5943Carbon TetrachlorideHCID 31398ChlorosuccinimideHCID 577431024-propyl-1-(1H-pyrrol-1-ylmethyl)pyrrolidin-2-one

생성물 1

HCID 577430721-[(2-chloro-1H-pyrrol-1-yl)methyl]-4-propylpyrrolidin-2-one수율 50%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

4-propyl-1-(1H-pyrrol-1-ylmethyl)pyrrolidin-2-one x264 (0.182 g, 0.88 mmol) is dissolved in absolute THF (3 ml). A solution of N-chlorosuccinimide (0.118 g, 1 eq) in absolute THF (1 ml) is added dropwise in a flow of argon at 0° C. The obtained solution is allowed to heat up slowly to room temperature in the cooling bath under stirring for 16 h. CCl4 (30 ml) is then added to the obtained solution. A small amount of a precipitate is filtered off, and the filtrate is evaporated. 1-[(2-chloro-1H-pyrrol-1-yl)methyl]-4-propylpyrrolidin-2-one 299 is isolated from the residue by reverse-phase HPLC (eluent: acetonitrile/water).

후처리

  1. filtrationA small amount of a precipitate is filtered off
  2. customthe filtrate is evaporated

출처 및 근거

ORD 기록
ord-85b2e192751f4d31b8e17b6f8a8846d6
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518943B2

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