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Methylamine → N~1~-[(4-Chlorophenyl)methyl]-N'~1~-methyl-2-nitroethene-1,1-diamine

HRID 1585037
ノート
印刷プレビュー

反応式

HRID 1585037 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][NH2:18]>CCO>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][NH:7][C:8]([NH:18][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 6329MethylamineHCID 70157188HCID 70157188、化合物

生成物 1

HCID 59896578N~1~-[(4-Chlorophenyl)methyl]-N'~1~-methyl-2-nitroethene-1,1-diamine収率 68.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

In 100 of EtOH on reflux was dissolved 2,59 g (0.01 mole) of 1-(4-chlorobenzyl) amino-1-methylthio-2-nitroethylene, and with refluxing continued, a solution of 1.49 g of 40% aqueous methylamine solution in 10 ml of EtOH was added cropwise over a period of 50 minutes. After completion of dropwise addition, the mixture was further refluxed for 15 minutes, at the end of which time it was cooled with ice-water, whereupon crystals separated out. The crystals were collected by filtration, washed with EtOH and ether in that order, and dried. The procedure gave 1.66 g of the title compound as white crystals.

後処理

  1. temperaturewith refluxing
  2. additionAfter completion of dropwise addition
  3. temperaturethe mixture was further refluxed for 15 minutes, at the end of which time it
  4. customseparated out
  5. filtrationThe crystals were collected by filtration
  6. washwashed with EtOH and ether in that order
  7. customdried

出典と根拠

ORDレコード
ord-fd4105b93e144c4b98c1529757b9c894
出典データセット
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05935981

反応ノート

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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