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Chloroform → HCID 12953064, 화합물

HRID 1577407
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HRID 1577407 반응식
[CH3:1][C:2]1[S:3][C:4]([CH3:19])=[C:5]2[C:10]=1[C:9](=[O:11])[N:8]1[CH:12]=[C:13]([C:16]([NH2:18])=O)[CH:14]=[CH:15][C:7]1=[N:6]2.P(Cl)(Cl)(Cl)=O.C(Cl)(Cl)Cl>N1C=CC=CC=1>[CH3:1][C:2]1[S:3][C:4]([CH3:19])=[C:5]2[C:10]=1[C:9](=[O:11])[N:8]1[CH:12]=[C:13]([C:16]#[N:18])[CH:14]=[CH:15][C:7]1=[N:6]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6212ChloroformHCID 24813Phosphorus oxychlorideHCID 12953063HCID 12953063, 화합물

생성물 1

HCID 12953064HCID 12953064, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

1,3-Dimethyl-10-oxo-10H-pyrido[1,2-a]thieno[3,4-d]pyrimidine-7-carboxamide (Example 50), 0.6 g (0.0022 mol), in 10 ml of pyridine, 25 ml of phosphorus oxychloride and 25 ml of chloroform is refluxed on a steam bath for two hours. The solvents are evaporated in vacuo and the residue is treated with 100 ml of water. The resulting precipitate is filtered to give 0.3 g of 1,3-dimethyl-10- oxo-10H-pyrido[1,2-a]thieno[3,4-d]pyrimidine-7-carbonitrile with methanol (1:0.125); mp 242°-244° C. after recrystallization from methanol.

후처리

  1. customThe solvents are evaporated in vacuo
  2. additionthe residue is treated with 100 ml of water
  3. filtrationThe resulting precipitate is filtered

출처 및 근거

ORD 기록
ord-96449e5a915343c6af8dd88f23ce1407
출처 데이터셋
uspto-grants-1981_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04287340

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