Chloroform → 2-methyl-10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carbonitrile

HRID 1577402ノート

反応式

HRID 1577402 の反応式
[CH3:1][C:2]1[S:10][C:9]2[C:8](=[O:11])[N:7]3[CH:12]=[C:13]([C:16]([NH2:18])=O)[CH:14]=[CH:15][C:6]3=[N:5][C:4]=2[CH:3]=1.P(Cl)(Cl)(Cl)=O.C(Cl)(Cl)Cl>N1C=CC=CC=1>[CH3:1][C:2]1[S:10][C:9]2[C:8](=[O:11])[N:7]3[CH:12]=[C:13]([C:16]#[N:18])[CH:14]=[CH:15][C:6]3=[N:5][C:4]=2[CH:3]=1

参加物

5

反応物 3

HCID 6212ChloroformHCID 24813Phosphorus oxychlorideHCID 129530542-methyl-10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carboxamide

生成物 1

HCID 129530552-methyl-10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carbonitrile

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

2-Methyl-10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carboxamide (Example 44), 0.6 g (0.0023 mol), in 10 ml of pyridine, 25 ml of phosphorus oxychloride and 25 ml of chloroform is refluxed on a steam bath for three hours. The solvents are evaporated in vacuo and the residue is treated with 100 ml of ice water. The resulting precipitate is filtered to give 0.5 g of 2-methyl-10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carbonitrile; mp 258°-259° C. after recrystallization from methanol.

後処理

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

出典と根拠

ORDレコード
ord-bc3e296b4e564550bd7cf32de070a7f9
出典データセット
uspto-grants-1981_09
特許番号
US04287340

反応ノート

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