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 1253181ノート

反応式

HRID 1253181 の反応式
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

参加物

4

反応物 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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e5177b493fd24c0696b670b6dd7caebc
出典データセット
uspto-grants-1988_05
特許番号
US04748175

反応ノート

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