Dichloromethane → methyl racemic-5-(4-hydroxy-1-piperidinyl)-2-oxo-2H-[1,2,4]oxadiazolo[2,3-a]pyrimidine-7-carbamate

HRID 26414ノート

反応式

HRID 26414 の反応式
[OH:1][CH:2]1[CH2:7][CH2:6][N:5]([C:8]2[N:13]=[C:12]([NH:14][C:15](OC)=[O:16])[N+:11]([O-:19])=[C:10]([NH:20][C:21]([O:23][CH3:24])=[O:22])[CH:9]=2)[CH2:4][CH2:3]1.C(Cl)Cl.[OH-].[Na+]>O>[OH:1][CH:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:9]=[C:10]([NH:20][C:21]([O:23][CH3:24])=[O:22])[N:11]3[O:19][C:15](=[O:16])[N:14]=[C:12]3[N:13]=2)[CH2:4][CH2:3]1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 178501992HCID 178501992、化合物

生成物 1

HCID 70605619methyl racemic-5-(4-hydroxy-1-piperidinyl)-2-oxo-2H-[1,2,4]oxadiazolo[2,3-a]pyrimidine-7-carbamate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

3.1 G. of dimethyl racemic-6-(4-hydroxy-1-piperidinyl)-2,4-pyrimidine-dicarbamate-3-oxide are suspended in 100 ml. of methylene chloride and 100 ml. of water. The suspension is adjusted with concentrated sodium hydroxide to pH 12.6 and stirred at this pH for 3.5 hours. The two phases are then separated and the aqueous phase is adjusted to pH 3.2 with concentrated hydrochloric acid solution. The separated white precipitate is filtered off, pre-dried and recrystallized from methylene chloride and methanol, there being obtained pure methyl racemic-5-(4-hydroxy-1-piperidinyl)-2-oxo-2H-[1,2,4]-oxadiazolo[2,3-a]pyrimidine-7-carbamate, having a melting point of 250°-260° C. (decomposition).

後処理

  1. customThe two phases are then separated
  2. filtrationThe separated white precipitate is filtered off
  3. custompre-dried
  4. customrecrystallized from methylene chloride and methanol, there

出典と根拠

ORDレコード
ord-bc81a90226344af0841c70fe7ba444a9
出典データセット
uspto-grants-1979_04
特許番号
US04150131

反応ノート

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