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

HRID 2043699ノート

反応式

HRID 2043699 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-794138a0464a455aae3994595c949796
出典データセット
uspto-grants-2013_11
特許番号
US08586623B2

反応ノート

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