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

HRID 249519
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HRID 249519 반응식
[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
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참가 물질

4

반응물 2

HCID 6329MethylamineHCID 70157188HCID 70157188, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

In 100 ml 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 1.94 g of 40% aqueous methylamine solution in 10 ml of EtOH was added dropwise 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.

후처리

  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

출처 및 근거

ORD 기록
ord-88b4ddfcf1bf404f9916189725e4ac3b
출처 데이터셋
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05214152

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