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Ammonia → HCID 25143769、化合物

HRID 1920497
ノート
印刷プレビュー

反応式

HRID 1920497 の反応式
[OH-].[K+].[C:3]([CH:5]([CH2:14][CH:15]([CH3:17])[CH3:16])[CH2:6][C:7]([N:9]([CH2:12][CH3:13])[CH2:10][CH3:11])=[O:8])#[N:4].N.[H][H]>CO.[Ni]>[NH2:4][CH2:3][CH:5]([CH2:14][CH:15]([CH3:17])[CH3:16])[CH2:6][C:7]([N:9]([CH2:12][CH3:13])[CH2:10][CH3:11])=[O:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 222AmmoniaHCID 14797Potassium HydroxideHCID 25143768HCID 25143768、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 25143769HCID 25143769、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol
溶媒

反応条件

温度
30 °C

実験手順

To a solution of potassium hydroxide (19 grams) in methanol (114 ml), 3-cyano-N,N-diethyl-5-methyl hexanamide (9.5 grams) was added followed by ammonia solution (38 ml) and Raney nickel (19 grams). Hydrogen pressure of 4.0 kg/cm2 was applied and the reaction mixture was stirred at 30° C. for 22 hours. The reaction mixture was filtered through a hyflow bed. The solvent was distilled off under reduced pressure at a temperature below 60° C. Water (200 ml) was added to the reaction mixture and pH adjusted to 2 with concentrated hydrochloric acid. The aqueous layer was extracted with dichloromethane. The pH of aqueous layer was adjusted to 8.0, with 50% sodium hydroxide. The aqueous layer was extracted with dichloromethane. The solvent was distilled off completely under atmospheric pressure to obtain the title compound as a residue.

後処理

  1. filtrationThe reaction mixture was filtered through a hyflow bed
  2. distillationThe solvent was distilled off under reduced pressure at a temperature below 60° C
  3. additionWater (200 ml) was added to the reaction mixture
  4. extractionThe aqueous layer was extracted with dichloromethane
  5. extractionThe aqueous layer was extracted with dichloromethane
  6. distillationThe solvent was distilled off completely under atmospheric pressure

出典と根拠

ORDレコード
ord-c4230f41c26440ed893876a921bc3041
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08168828B2

反応ノート

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