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

HRID 1926850ノート

反応式

HRID 1926850 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-0ec9c617408a45408fdd924f6e0dc801
出典データセット
uspto-grants-2012_05
特許番号
US08183241B2

反応ノート

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