Gamma-Butyrolactone → HCID 20340747, 화합물

HRID 1395261노트

반응식

[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

참가 물질

반응물 3

HCID 7302Gamma-Butyrolactone

HCID 11430Potassium Carbonate

HCID 129098391,2-Diaminopyridinium iodide

생성물 1

HCID 20340747HCID 20340747, 화합물

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록: ord-88bfdba64b354e7999cf098a7ee5a1ba
출처 데이터셋: uspto-grants-1980_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04202977

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