Gamma-Butyrolactone → HCID 20340747、化合物

HRID 1395261ノート

反応式

HRID 1395261 の反応式
[I-].[NH2:2][N+:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH2:9].[C:10]1(=O)[O:14][CH2:13][CH2:12][CH2:11]1.C(=O)([O-])[O-].[K+].[K+]>>[OH:14][CH2:13][CH2:12][CH2:11][C:10]1[N:9]=[C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][N:3]2[N:2]=1

参加物

4

反応物 3

HCID 7302Gamma-ButyrolactoneHCID 11430Potassium CarbonateHCID 129098391,2-Diaminopyridinium iodide

生成物 1

HCID 20340747HCID 20340747、化合物

実験手順

A mixture of 24 g of 1,2-diaminopyridinium iodide, 17.2 g of γ-butyrolactone and 57 g of potassium carbonate in 100 ml of diethylcellosolve was refluxed with stirring for 8 hours. The mixture was concentrated under reduced pressure to the residue, which was extracted by hot dichloromethane. The solvent was removed to give crude 2-(3-hydroxypropyl)-s-triazolo[1,5-a]pyridine, which was recrystallized from ethyl acetate to colorless needles (16 g, 90%), mp 71.5°-73° C. Anal. Calcd. for C9H11ON3 : C, 61.00; H, 6.24; N, 23.72. Found: C, 60.82; H, 6.14; N, 23.48.

後処理

  1. temperaturewas refluxed
  2. concentrationThe mixture was concentrated under reduced pressure to the residue, which
  3. extractionwas extracted by hot dichloromethane
  4. customThe solvent was removed

出典と根拠

ORDレコード
ord-88bfdba64b354e7999cf098a7ee5a1ba
出典データセット
uspto-grants-1980_05
特許番号
US04202977

反応ノート

読み込み中…