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Dimethyl Sulfoxide → HCID 44602516、化合物

HRID 448540
ノート
印刷プレビュー

反応式

HRID 448540 の反応式
C(Cl)(=O)C(Cl)=O.CS(C)=O.[Cl:11][CH2:12][CH2:13][C:14]1[C:19](=[O:20])[N:18]2[CH2:21][CH2:22][CH2:23][CH:24]([OH:25])[C:17]2=[N:16][C:15]=1[CH3:26].C(N(CC)CC)C>ClCCl>[Cl:11][CH2:12][CH2:13][C:14]1[C:19](=[O:20])[N:18]2[CH2:21][CH2:22][CH2:23][C:24](=[O:25])[C:17]2=[N:16][C:15]=1[CH3:26]
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 679Dimethyl SulfoxideHCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 155471943-(2-Chloroethyl)-6,7,8,9-tetrahydro-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

生成物 1

HCID 44602516HCID 44602516、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

A solution of oxalylchloride (8.8 ml) in dichloromethane (20 ml) was cooled to −65° C. and a solution of dimethyl sulfoxide (6.5 ml) dissolved in dichloromethane (20 ml) was added to it slowly and stirred for 30 min. keeping the temperature at −65° C. a solution of 3-(2-chloroethyl)-9-hydroxy-2-methyl-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidin-4-one (5 grams) (formula-7) dissolved in dichloromethane (30 ml) was added to it very slowly and stirred for 40 min. Triethyl amine was added to the reaction mixture and then quenched with water. The organic layer was separated, washed with aqueous sodium carbonate and water. The solvent from the organic layer was distilled off under reduced pressure to provide the title compound.

後処理

  1. additionwas added to it slowly
  2. customat −65° C.
  3. additionwas added to it very slowly
  4. stirringstirred for 40 min
  5. customquenched with water
  6. customThe organic layer was separated
  7. washwashed with aqueous sodium carbonate and water
  8. distillationThe solvent from the organic layer was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-0768b6b37ae74e278e21280929a41dd7
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08481729B2

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