Ethyl Acetate → HCID 178469959、化合物

HRID 900894

反応式

HRID 900894 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH2:9][C:10]([O:12]CC)=O)=[CH:4][CH:3]=1.[NH2:16][C:17]1[NH:21][N:20]=[CH:19][C:18]=1[C:22]([O:24][CH2:25][CH3:26])=[O:23].CCOC(C)=O>CCCCCC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[C:10]([OH:12])[N:21]3[N:20]=[CH:19][C:18]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[C:17]3[N:16]=2)=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 81472ethyl 3-amino-1H-pyrazole-4-carboxylateHCID 101336Ethyl 3-(4-chlorophenyl)-3-oxopropanoate

生成物 1

HCID 178469959HCID 178469959、化合物収率 52.3%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

反応条件

温度
160 °C

実験手順

A mixture of ethyl 3-(4-chloro-phenyl)-3-oxo-propionate (18.1 g, 0.080 mol) and ethyl 5-amino-1H-pyrazole-4-carboxylate (13.7 g, 0.088 mol) was stirred at 160° C. for 3 h. AcOEt (40 mL) and hexane (40 mL) were successively added to the cooled mixture and stirring was continued at 0° C. for 0.5 h. The crystals were isolated by filtration and the solid was triturated for 1.2 h with 0.2 N HCl (80 mL). The solid was filtered off, washed with water and dried to give ethyl 5-(4-chloro-phenyl)-7-hydroxy-pyrazolo[1,5-a]pyrimidine-3-carboxylate (13.3 g, 52%). White solid. MS (ISN) 316.3 [(M−H)−]; mp 190-192° C.

後処理

  1. stirringstirring
  2. waitwas continued at 0° C. for 0.5 h
  3. customThe crystals were isolated by filtration
  4. customthe solid was triturated for 1.2 h with 0.2 N HCl (80 mL)
  5. filtrationThe solid was filtered off
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-b1c661d8ec6f49b7ab0ed483554dcefa
出典データセット
uspto-grants-2008_04
特許番号
US07361659B2

関連ノート

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