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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 12888773, 화합물 → HCID 135759095, 화합물

HRID 1995281
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HRID 1995281 반응식
[CH3:1][N:2]1[CH:6]=[C:5]([C:7]#[N:8])[C:4]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=2[N+:17]([O-])=O)=[N:3]1>C(O)C.Cl>[NH2:8][C:7]1[C:5]2[C:4](=[N:3][N:2]([CH3:1])[CH:6]=2)[NH:9][C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][C:11]=2[N:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 12888773HCID 12888773, 화합물

생성물 1

HCID 135759095HCID 135759095, 화합물

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

To 1-methyl-3-(4-chloro-2-nitroanilino)pyrazole-4-carbonitrile (16 g) stirred in ethanol (500 ml) was added a solution of anhydrous stannous chloride (33.1 g) in concentrated hydrochloric acid (176 ml). The mixture was heated under reflux for 2 hours, cooled, filtered and crystallised from methylated spirits (1 liter) to give the title compound as its hydrochloride salt m.p. >260° C. 2.0 g of the hydrochloride salt was partitioned between dilute ammonia solution and chloroform. The organic phase was washed with water, dried with magnesium sulphate, evaporated and the residue crystallised from chloroform-n-hexane to give the title compound as the free base m.p. 240° C.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. temperaturecooled
  4. filtrationfiltered
  5. customcrystallised from methylated spirits (1 liter)

출처 및 근거

ORD 기록
ord-5f76fefde02e41de8dfeb70b219e811c
출처 데이터셋
uspto-grants-1983_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04404137

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