Phosphorus oxychloride → 5-Chloro-1,6-naphthyridine

반응식

[N:1]1[C:10]2[CH:9]=[CH:8][N:7]=[C:6](O)[C:5]=2[CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:6]1[N:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[CH:4]=[CH:3][CH:2]=[N:1]2

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 178517692HCID 178517692, 화합물

생성물 1

HCID 122042345-Chloro-1,6-naphthyridine수율 87%

반응 조건

온도: 80 °C

실험 절차

The product from Example 36d (0.250 g, 1.71 mmol) was combined with phosphorous oxychloride (4 mL) and heated under a nitrogen atmosphere at 80° C. for 18.5 h followed by vacuum distillation to remove the volatiles. The residue was slurried with ice and made basic (pH 7-8) with concentrated ammonium hydroxide. The title compound was collected by vacuum filtration, water washed and dried under vacuum to give a gray solid (0.245 g, 87%) sufficiently pure for use as isolated.

후처리

distillationfollowed by vacuum distillation
customto remove the volatiles
filtrationThe title compound was collected by vacuum filtration, water
washwashed
customdried under vacuum

출처 및 근거

ORD 기록: ord-37b0ea41be9c41638601733c59d369dd
출처 데이터셋: uspto-grants-2012_08
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08236950B2

반응 노트

불러오는 중…