Triethylamine → 4-(Pyrrolidin-1-yl)-2,5-difluorobenzoic acid ethyl ester

HRID 729372ノート

反応式

HRID 729372 の反応式
[CH2:1]([O:3][C:4](=[O:14])[C:5]1[CH:10]=[C:9]([F:11])[C:8](F)=[CH:7][C:6]=1[F:13])[CH3:2].[CH2:15]([N:17](CC)[CH2:18][CH3:19])[CH3:16].N1CCCC1>C(#N)C.C(OCC)(=O)C>[CH2:1]([O:3][C:4](=[O:14])[C:5]1[CH:10]=[C:9]([F:11])[C:8]([N:17]2[CH2:18][CH2:19][CH2:16][CH2:15]2)=[CH:7][C:6]=1[F:13])[CH3:2]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 31268PyrrolidineHCID 2774397Benzoic acid, 2,4,5-trifluoro-, ethyl ester

生成物 1

HCID 210411804-(Pyrrolidin-1-yl)-2,5-difluorobenzoic acid ethyl ester収率 97%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2,4,5-trifluorobenzoic acid ethyl ester (Example 1e, 4.32 g, 21.2 mmol) in acetonitrile (25 mL) is added triethylamine (5.9 mL, 42.3 mmol) and pyrrolidine (2.2 mL, 25.4 mmol). After 24 hours, the reaction mixture is diluted with ethyl acetate and washed with saturated NaHCO3, water, and brine. The organic layer is dried over MgSO4, filtered, and the filtrate is concentrated to afford the title compound as an oil (5.25 g). MS CI: m/z 256 (MH+).

後処理

  1. washwashed with saturated NaHCO3, water, and brine
  2. dry with materialThe organic layer is dried over MgSO4
  3. filtrationfiltered
  4. concentrationthe filtrate is concentrated

出典と根拠

ORDレコード
ord-7b108041613441d4a79047de8c2bfc4c
出典データセット
uspto-grants-2009_09
特許番号
US07582627B2

反応ノート

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