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Dimethylamine → HCID 59896602、化合物

HRID 1682234
ノート
印刷プレビュー

反応式

HRID 1682234 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][NH:7][C:8](SC)=[CH:9][N+:10]([O-:12])=[O:11])=[CH:4][CH:3]=1.[CH3:17][NH:18][CH3:19]>CCO>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][NH:7][C:8]([N:18]([CH3:19])[CH3:17])=[CH:9][N+:10]([O-:12])=[O:11])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 674DimethylamineHCID 70157188HCID 70157188、化合物

生成物 1

HCID 59896602HCID 59896602、化合物収率 47.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

In 100 ml of EtOH was dissolved 2.59 g (0.01 mole) of 1-(4-chlorobenzyl)amino-1-methylthio-2-nitroethylene with heating. Then, with refluxing and stirring, a solution of 2.25 g of 50% aqueous dimethylamine solution in 10 ml of EtOH was added dropwise over a period of 35 minutes. After completion of dropwise addition, the mixture was further stirred and refluxed for 2.5 hours. The solvent was then distilled off and the residue was diluted with ether and triturated, whereupon crystals separated. After addition of EtOH and ether (about 1:5), the crystals were collected by filtration, washed with ether and dried. The procedure gave 1.21 g of the title compound as white crystals.

後処理

  1. temperaturewith heating
  2. temperatureThen, with refluxing
  3. additionAfter completion of dropwise addition
  4. stirringthe mixture was further stirred
  5. temperaturerefluxed for 2.5 hours
  6. distillationThe solvent was then distilled off
  7. additionthe residue was diluted with ether
  8. customtriturated, whereupon crystals
  9. customseparated
  10. additionAfter addition of EtOH and ether (about 1:5)
  11. filtrationthe crystals were collected by filtration
  12. washwashed with ether
  13. customdried

出典と根拠

ORDレコード
ord-c3da7b75817a467e91292b0d2b50a48d
出典データセット
uspto-grants-1992_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05175301

反応ノート

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