Ethanol → HCID 178470502、化合物

HRID 652094

反応式

HRID 652094 の反応式
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([C:7]([O:9][CH3:10])=[O:8])[N:3]=1.[N:11]1([CH2:17][C:18]2[CH:19]=[C:20]([CH:27]=[CH:28][CH:29]=2)[O:21][CH2:22][CH2:23][CH2:24][CH:25]=O)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1.[BH4-].[Na+].[CH2:32](O)C>>[N:11]1([CH2:17][C:18]2[CH:19]=[C:20]([CH:27]=[CH:28][CH:29]=2)[O:21][CH2:22][CH2:23][CH2:24][CH2:25][NH:1][C:2]2[NH:6][N:5]=[C:4]([C:7]([O:9][CH2:10][CH3:32])=[O:8])[N:3]=2)[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1

参加物

5

反応物 4

HCID 702EthanolHCID 4311764Sodium borohydrideHCID 212975474-[3-(1-Piperidinylmethyl)phenoxy]butanalHCID 178499187HCID 178499187、化合物

生成物 1

HCID 178470502HCID 178470502、化合物

実験手順

Methyl 5-amino-1H-1,2,4-triazole-3-carboxylate (0.568 g) and 4-[3-(1-piperidinylmethyl)phenoxy]butanal in ethanol (40 ml were heated at reflux for 2 h. The cooled reaction mixture was treated with sodium borohydride (0.4 g) and stirred at room temperature for 15 h. The solvent was evaporated and the residue was dissolved in 2N hydrochloric acid which was washed with ethyl acetate, basified with sodium carbonate and extracted with ethyl acetate. The combined organic extracts were evaporated to yield the title compound as a white solid which was recrystallised from a mixture of ethyl acetate and ethanol (1:1) (0.5 g) m.p. 170°-1° dec.

後処理

  1. temperatureat reflux for 2 h
  2. customThe cooled reaction mixture
  3. customThe solvent was evaporated
  4. dissolutionthe residue was dissolved in 2N hydrochloric acid which
  5. washwas washed with ethyl acetate
  6. extractionextracted with ethyl acetate
  7. customThe combined organic extracts were evaporated

出典と根拠

ORDレコード
ord-bf9d655a40df4ec2b3af3137ab978e47
出典データセット
uspto-grants-1987_06
特許番号
US04670448

関連ノート

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