1-Butanol → 2,6-Dimethyl-4-[4-(2-hydroxyethyl)-1-piperazinyl]-6,7-dihydro-8H-pyrimido[5,4-b][1,4]oxazin-7-one

HRID 1253181노트

반응식

HRID 1253181 반응식
Cl[C:2]1[C:7]2[O:8][CH:9]([CH3:13])[C:10](=[O:12])[NH:11][C:6]=2[N:5]=[C:4]([CH3:14])[N:3]=1.O[CH:16]([N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1)[CH3:17].C([OH:28])CCC>>[CH3:14][C:4]1[N:3]=[C:2]([N:21]2[CH2:22][CH2:23][N:18]([CH2:16][CH2:17][OH:28])[CH2:19][CH2:20]2)[C:7]2[O:8][CH:9]([CH3:13])[C:10](=[O:12])[NH:11][C:6]=2[N:5]=1

참가 물질

4

반응물 3

HCID 2631-ButanolHCID 36767354-chloro-2,6-dimethyl-6,7-dihydro-8H-pyrimido[5,4-b][1,4]oxazin-7-oneHCID 177695631-(Piperazin-1-yl)ethan-1-ol

생성물 1

HCID 201372972,6-Dimethyl-4-[4-(2-hydroxyethyl)-1-piperazinyl]-6,7-dihydro-8H-pyrimido[5,4-b][1,4]oxazin-7-one

실험 절차

A mixture containing 0.86 g of 4-chloro-2,6-dimethyl-6,7-dihydro-8H-pyrimido[5,4-b][1,4]oxazin-7-one (Khim. Geterotsikl. Soed. 1972, 1285), 20 ml of n-butanol and 1.04 g of 1-hydroxyethylpiperazine is refluxed for 7 hours, then evaporated. After adding 20 ml of water, the residue is extracted with ethyl acetate. The organic solution is dried and evaporated. After recrystallizing the residue from ethyl acetate, 0.90 g of product is obtained, m.p.: 160°-161° C.

후처리

  1. temperatureis refluxed for 7 hours
  2. customevaporated
  3. additionAfter adding 20 ml of water
  4. extractionthe residue is extracted with ethyl acetate
  5. customThe organic solution is dried
  6. customevaporated
  7. customAfter recrystallizing the residue from ethyl acetate

출처 및 근거

ORD 기록
ord-e5177b493fd24c0696b670b6dd7caebc
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04748175

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