Potassium Carbonate → HCID 22509303, 화합물

HRID 984876노트

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HRID 984876 반응식
Cl[C:2]1[N:7]=[CH:6][C:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:4][N:3]=1.[C:13]([C:17]1[CH:18]=[C:19]([CH:21]=[C:22]([C:24]([CH3:27])([CH3:26])[CH3:25])[CH:23]=1)[NH2:20])([CH3:16])([CH3:15])[CH3:14].C([O-])([O-])=O.[K+].[K+]>O>[C:24]([C:22]1[CH:21]=[C:19]([NH:20][C:2]2[N:7]=[CH:6][C:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:4][N:3]=2)[CH:18]=[C:17]([C:13]([CH3:16])([CH3:15])[CH3:14])[CH:23]=1)([CH3:27])([CH3:26])[CH3:25]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 754193,5-Di-tert-butylanilineHCID 104878152-Chloro-pyrimidine-5-carboxylic acid ethyl ester

생성물 1

HCID 22509303HCID 22509303, 화합물수율 90%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
110 °C

실험 절차

A mixture of ethyl 2-chloropyrimidine-5-carboxylate (335 mg), 3,5-di-tert-butylaniline (370 mg), and K2CO3 (600 mg) was heated at 110° C. After the disappearance of the materials was observed with TLC, the reaction mixture was poured into water, and extracted with CH2Cl2. The organic layer was dried over Na2SO4, and the solvent was evaporated. The residue was purified by silica gel flash column chromatography (n-hexane: AcOEt=10:1) to give white crystals of ethyl 2-[N-(3,5-di-tert-butylphenyl)amino]pyrimidine-5-carboxylate (574 mg, 90%).

후처리

  1. extractionextracted with CH2Cl2
  2. dry with materialThe organic layer was dried over Na2SO4
  3. customthe solvent was evaporated
  4. customThe residue was purified by silica gel flash column chromatography (n-hexane: AcOEt=10:1)

출처 및 근거

ORD 기록
ord-7e4ed6b11c3048eaa311080f6a7276d1
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06869959B1

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