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N-((6-chloro-3-pyridinyl)methyl)-1,2-ethane-diamine → HCID 72727592, 화합물

HRID 1382227
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HRID 1382227 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][CH2:10][CH2:11][NH2:12])=[CH:4][N:3]=1.[N+:13]([CH2:16][C:17](SC)=[S:18])([O-:15])=[O:14]>CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][CH2:10][CH2:11][NH:12][C:17]([SH:18])=[CH:16][N+:13]([O-:15])=[O:14])=[CH:4][N:3]=1
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참가 물질

4

반응물 2

HCID 10997737N-((6-chloro-3-pyridinyl)methyl)-1,2-ethane-diamineHCID 14653529HCID 14653529, 화합물

생성물 1

HCID 72727592HCID 72727592, 화합물수율 38.6%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
50 °C

실험 절차

N-(2-chloro-5-pyridylmethyl)ethylenediamine (2.0 g) and methyl 2-nitrodithioacetate (1.7 g) were dissolved in methanol (40 ml), and the solution was heated at 50° C. for 1 hour in a stream of nitrogen. The solution was cooled to room temperature whereupon crystals were precipitated. The crystals were collected by filtration, washed with a small amount of methanol, and then dried to give the desired N-(2-chloro-5-pyridylmethyl)-N'-(1-mercapto-2-nitrovinyl)ethylenediamine (1.2 g) having a melting point of 136° to 137° C. (decomp.).

후처리

  1. temperatureThe solution was cooled to room temperature whereupon crystals
  2. customwere precipitated
  3. filtrationThe crystals were collected by filtration
  4. washwashed with a small amount of methanol
  5. customdried

출처 및 근거

ORD 기록
ord-26ca90fa4e254a2998a2105bd18d18e5
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04806553

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