Sodium Hydroxide → HCID 178467457、化合物

HRID 542385ノート

反応式

HRID 542385 の反応式
[CH3:1][N:2]([CH3:17])[C:3]1[C:8]([NH:9][C:10](=[O:13])[CH2:11][Cl:12])=[C:7]([O:14][CH2:15][CH3:16])[N:6]=[CH:5][N:4]=1.Cl.[NH:19]1[CH:23]=[CH:22][C:21]([CH2:24]Cl)=[N:20]1.[OH-].[Na+]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.C(Cl)Cl.O>[NH:19]1[CH:23]=[CH:22][C:21]([CH2:24][N:9]([C:8]2[C:3]([N:2]([CH3:17])[CH3:1])=[N:4][CH:5]=[N:6][C:7]=2[O:14][CH2:15][CH3:16])[C:10](=[O:13])[CH2:11][Cl:12])=[N:20]1

参加物

7

反応物 3

HCID 14798Sodium HydroxideHCID 20208140N-(4-dimethylamino-6-ethoxypyrimidin-5-yl)-chloroacetamideHCID 178478564HCID 178478564、化合物

生成物 1

HCID 178467457HCID 178467457、化合物

試薬・触媒・溶媒 3

HCID 66133Benzyl triethylammonium chloride触媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a mixture of 12.9 g (0.05 mol) N-(4-dimethylamino-6-ethoxypyrimidin-5-yl)-chloroacetamide and 2 g benzyltriethylammoniumchloride in 150 g of CH2Cl2 are added 8.4 g (0.055 mol) of 1-pyrazolylmethylchloride-hydrochloride. To this mixture are quickly added 25 ml of 40% NaOH, whereby the temperature rises from 18° to 32°. The mixture is then stirred for 2 hours and diluted with water. The organic phase is separated off and dried over Na2SO4. The dried solution is evaporated to give an orange oil that is chromatographed on silica gel with the aid of ethylacetate. The thus obtained yellow oil is dissolved in diethylether and crystallised in a deep-freezer. The title compound is obtained in the form of white crystals of m.p. 112°-114°.

後処理

  1. customrises from 18° to 32°
  2. customThe organic phase is separated off
  3. dry with materialdried over Na2SO4
  4. customThe dried solution is evaporated
  5. customto give an orange oil that
  6. customis chromatographed on silica gel with the aid of ethylacetate
  7. dissolutionThe thus obtained yellow oil is dissolved in diethylether
  8. customcrystallised in a deep-freezer

出典と根拠

ORDレコード
ord-ef3746e0b2784720a0954597e16b8c31
出典データセット
uspto-grants-1987_04
特許番号
US04657579

反応ノート

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