Sodium Hydroxide → HCID 178467457, 화합물

HRID 542385노트

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HRID 542385 반응식
[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

참가 물질

7

반응물 3

HCID 14798Sodium HydroxideHCID 20208140N-(4-dimethylamino-6-ethoxypyrimidin-5-yl)-chloroacetamideHCID 178478564HCID 178478564, 화합물

생성물 1

HCID 178467457HCID 178467457, 화합물

시약·촉매·용매 3

HCID 66133Benzyl triethylammonium chloride촉매HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-ef3746e0b2784720a0954597e16b8c31
출처 데이터셋
uspto-grants-1987_04
특허 번호
US04657579

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