Water → HCID 20237825、化合物

HRID 365196ノート

反応式

HRID 365196 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 20237825HCID 20237825、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-df68696b9e5246bbb82e13a148c23586
出典データセット
uspto-grants-1986_08
特許番号
US04608383

反応ノート

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