Water → HCID 20237825, 화합물

HRID 1903795노트

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HRID 1903795 반응식
Cl[C:2]1[N:3]([CH3:12])[C:4](=[O:11])[N:5]([CH3:10])[C:6](=[O:9])[C:7]=1[CH3:8].[O:13]([CH2:20][CH:21]([OH:30])[CH2:22][NH:23][CH2:24][C:25]([CH3:29])([CH3:28])[CH2:26][NH2:27])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.N1C=CC=CC=1.O>C(Cl)Cl>[O:13]([CH2:20][CH:21]([OH:30])[CH2:22][NH:23][CH2:24][C:25]([CH3:28])([CH3:29])[CH2:26][NH:27][C:2]1[N:3]([CH3:12])[C:4](=[O:11])[N:5]([CH3:10])[C:6](=[O:9])[C:7]=1[CH3:8])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 132969876-Chloro-1,3,5-trimethyl-2,4(1H,3H)-pyrimidinedioneHCID 20237895HCID 20237895, 화합물

생성물 1

HCID 20237825HCID 20237825, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4.5 g. 4-Chloro-1,3,5-trimethylpyrimidine-2,6(1H,3H)-dione and 6.1 g. 1-phenoxy-3-(3-amino-2,2-dimethylpropylamino)-propan-2-ol (b.p. 159°-161° C./0.01 mm.Hg; obtained from phenyl glycidyl ether and 2,2-dimethyl-1,3-diaminopropane) are stirred for 50 hours at 80° C. in 8 ml. pyridine. The reaction mixture is taken up in methylene chloride, shaken with water, dried, evaporated and the residue obtained chromatographed on silica gel in the manner described in Example 29 to give 2.3 g. (24% of theory) of the desired product in the form of colorless crystals; m.p. 111°-112° C., after recrystallization from ethyl acetate.

후처리

  1. customdried
  2. customevaporated
  3. customthe residue obtained
  4. customchromatographed on silica gel in the manner
  5. customto give 2.3 g

출처 및 근거

ORD 기록
ord-252e6ae5232e4b07a41f6e197b8126a1
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04438128

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