Sodium Chloride → N-[1-(3-methyl-4-nitrophenyl)pyrrolidin-3-yl]acetamide

HRID 349133ノート

反応式

HRID 349133 の反応式
F[C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([CH3:8])[CH:7]=1.[C:12]([NH:15][CH:16]1[CH2:20][CH2:19][NH:18][CH2:17]1)(=[O:14])[CH3:13].C(=O)([O-])[O-].[K+].[K+].[Cl-].[Na+]>CN1C(=O)CCC1>[CH3:8][C:6]1[CH:7]=[C:2]([N:18]2[CH2:19][CH2:20][CH:16]([NH:15][C:12](=[O:14])[CH3:13])[CH2:17]2)[CH:3]=[CH:4][C:5]=1[N+:9]([O-:11])=[O:10]

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 11430Potassium CarbonateHCID 949565-Fluoro-2-nitrotolueneHCID 5227153-Acetamidopyrrolidine

生成物 1

HCID 21087633N-[1-(3-methyl-4-nitrophenyl)pyrrolidin-3-yl]acetamide収率 98%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
95 °C

実験手順

After dissolving 15.5 g of 5-fluoro-2-nitrotoluene (0.1 mol) and 12.8 g of 3-acetamido-pyrrolidine (0.1 mol) in 75 ml of NMP, 15.8 g of potassium carbonate (0.12 mol) are added under a nitrogen atmosphere and the mixture is heated at 95° C. for 20 h. The reaction medium is allowed to cool and is then poured into 600 ml of saturated aqueous sodium chloride solution. The yellow precipitate formed is filtered off, washed with 15% NaCl solution until a pH equal to 7 is obtained for the washing waters, and washed with petroleum ether and then dried in a vacuum oven over P2O5. 25.7 g (98%) of N-[1-(3-methyl-4-nitrophenyl)pyrrolidin-3-yl]acetamide are thus obtained in the form of a yellow solid.

後処理

  1. additionare added under a nitrogen atmosphere
  2. temperatureto cool
  3. customThe yellow precipitate formed
  4. filtrationis filtered off
  5. washwashed with 15% NaCl solution until a pH equal to 7
  6. customis obtained for the washing waters
  7. washwashed with petroleum ether
  8. dry with materialdried in a vacuum oven over P2O5

出典と根拠

ORDレコード
ord-c9034cd525284aab92e2d40aa38021b4
出典データセット
uspto-grants-2007_02
特許番号
US07179301B2

反応ノート

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