ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Dimethylformamide → HCID 89875881、化合物

HRID 1048634
ノート
印刷プレビュー

反応式

HRID 1048634 の反応式
[CH3:1][C:2]1[C:7]([O:8][CH2:9][CH3:10])=[CH:6][CH:5]=[CH:4][C:3]=1[N:11]1[C:15](=[O:16])[NH:14][N:13]=[N:12]1.[C:17](=O)([O-])[O-].[K+].[K+].CN(C)C=O.S(OC)(OC)(=O)=O>O>[CH3:1][C:2]1[C:7]([O:8][CH2:9][CH3:10])=[CH:6][CH:5]=[CH:4][C:3]=1[N:11]1[C:15](=[O:16])[N:14]([CH3:17])[N:13]=[N:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 136646183HCID 136646183、化合物

生成物 1

HCID 89875881HCID 89875881、化合物収率 92.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Under ice-cooling, to a mixture of 1-(2-methyl-3-ethoxyphenyl)-1,4-dihydrotetrazole-5-one 39.0 g, potassium carbonate 36.7 g and N,N-dimethylformamide 400 mL was added dimethyl sulfate 44.7 g and the resulting mixtures were raised to room temperature and were stirred for seven hours. Thereto was added water and the mixtures were extracted with ethyl acetate and the organic layers were washed with water and saturated saline, and were dried over anhydrous magnesium sulfate and were then concentrated under reduced pressure. The resulting residues were subjected to a silica gel column chromatography to give 1-(2-methyl-3-ethoxyphenyl)-4-methyl-1,4-dihydrotetrazole-5-one 38.2 g.

後処理

  1. extractionthe mixtures were extracted with ethyl acetate
  2. washthe organic layers were washed with water and saturated saline
  3. dry with materialwere dried over anhydrous magnesium sulfate
  4. concentrationwere then concentrated under reduced pressure

出典と根拠

ORDレコード
ord-8d0888b8740646e186ceb30047fdf103
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09380782B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート