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1,1'-Carbonyldiimidazole → HCID 178438393、化合物

HRID 1155875
ノート
印刷プレビュー

反応式

HRID 1155875 の反応式
[CH3:1][CH:2]([C:4]1[S:20][C:7]2[N:8]=[C:9]3[CH:16]=[CH:15][C:14]([C:17](O)=[O:18])=[CH:13][N:10]3[C:11](=[O:12])[C:6]=2[CH:5]=1)[CH3:3].C(N1C=CN=C1)(N1C=CN=C1)=O.O.[NH2:34][C:35]1[NH:39][N:38]=[N:37][N:36]=1>CN(C)C=O>[CH3:3][CH:2]([C:4]1[S:20][C:7]2[N:8]=[C:9]3[CH:16]=[CH:15][C:14]([C:17]([NH:34][C:35]4[NH:39][N:38]=[N:37][N:36]=4)=[O:18])=[CH:13][N:10]3[C:11](=[O:12])[C:6]=2[CH:5]=1)[CH3:1]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 682631,1'-CarbonyldiimidazoleHCID 12862353HCID 12862353、化合物HCID 178509300HCID 178509300、化合物

生成物 1

HCID 178438393HCID 178438393、化合物収率 50.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
105 °C

実験手順

2.88 g (0.01 mol) of 2-(1-methylethyl)-4-oxo-4H-pyrido[1,2-a]thieno[2,3-d]pyrimidin-7-carboxylic acid (Example 18) and 3.31 g (0.02 mol) of 1,1' carbonyldiimidazole (Aldrich Chemical Company) in 100 ml of dimethylformamide are stirred and heated in a wax bath at 105° C. for ninety minutes under nitrogen. The mixture is cooled and stirred at room temperature for thirty minutes and 1.03 g (0.01 mol) of 5-aminotetrazole monohydrate (Aldrich Chemical Company) is added and the resulting mixture is stirred and heated at 105° C. for one hundred thirty-five minutes under nitrogen. The mixture is allowed to stand overnight at room temperature, the precipitate is filtered and the filtrate is evaporated in vacuo. The residue is slurried in boiling methanol, the mixture cooled and filtered. This precipitate is combined with the previous precipitate to give 1.8 g of 2-(1-methylethyl)-4-oxo-N-1H-tetrazol-5-yl-4H-pyrido[1,2-a]thieno[2,3-d]pyrimidine-7 -carboxamide; mp 307° C. (dec) after recrystallization from pyridine.

後処理

  1. temperatureThe mixture is cooled
  2. stirringthe resulting mixture is stirred
  3. temperatureheated at 105° C. for one hundred thirty-five minutes under nitrogen
  4. filtrationthe precipitate is filtered
  5. customthe filtrate is evaporated in vacuo
  6. temperaturethe mixture cooled
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-d21c1d43efa942edb708db7e81b3a7fd
出典データセット
uspto-grants-1982_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04332947

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート