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Dimethylamine → 1-(6-Chloro-3-pyridylmethyl)3,3-dimethyl-2-nitroguanidine

HRID 728990
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HRID 728990 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][C:10](=[N:13][N+:14]([O-:16])=[O:15])SC)=[CH:4][N:3]=1.[CH3:17][NH:18][CH3:19]>C(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][C:10](=[N:13][N+:14]([O-:16])=[O:15])[N:18]([CH3:19])[CH3:17])=[CH:4][N:3]=1
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참가 물질

4

반응물 2

HCID 674DimethylamineHCID 1361361971-(2-Chloro-5-pyridylmethyl)-2-methyl-3-nitroisothiourea

생성물 1

HCID 1362181971-(6-Chloro-3-pyridylmethyl)3,3-dimethyl-2-nitroguanidine수율 93.4%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
30 °C

실험 절차

1-(2-chloro-5-pyridylmethyl)-2-methyl-3-nitroisothiourea (1.3 g) was dissolved in ethanol (20 ml) and to the solution was added an aqueous solution (50%) of dimethylamine (0.5 g) at room temperature, followed by one-day stirring at 30° C. The ethanol in the solution was distilled off under reduced pressure and it was purified on a chromatographic column (the eluent was a mixture of methanol and chloroform) so as to obtain the desired 3-(2-chloro-5-pyridylmethyl)-1,1-dimethyl-2-nitroguanidine (1.2 g) having a melting point in the range of from 158° to 160° C.

후처리

  1. waitfollowed by one-day
  2. distillationThe ethanol in the solution was distilled off under reduced pressure and it
  3. customwas purified on a chromatographic column (the eluent
  4. additiona mixture of methanol and chloroform) so as

출처 및 근거

ORD 기록
ord-16119633672448cab3b2625b1e6c953b
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05051434

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