HCID 71766083, 화합물 → HCID 71766225, 화합물

HRID 403378노트

반응식

HRID 403378 반응식
ClC1N=NC(NC)=C(C2C=CC=CC=2)C=1.[Cl:16][C:17]1[N:22]=[N:21][C:20]([N:23]([CH3:40])[C:24](=[O:39])[C:25]2[CH:30]=[C:29]([C:31]([F:34])([F:33])[F:32])[CH:28]=[C:27]([S:35]([CH3:38])(=[O:37])=[O:36])[CH:26]=2)=[C:19]([C:41]2[CH:46]=[CH:45][C:44](F)=[CH:43][C:42]=2OC)[CH:18]=1>CCCCCCC.C(OCC)(=O)C>[Cl:16][C:17]1[N:22]=[N:21][C:20]([N:23]([CH3:40])[C:24](=[O:39])[C:25]2[CH:30]=[C:29]([C:31]([F:34])([F:32])[F:33])[CH:28]=[C:27]([S:35]([CH3:38])(=[O:36])=[O:37])[CH:26]=2)=[C:19]([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[CH:18]=1

참가 물질

4

반응물 2

HCID 71766083HCID 71766083, 화합물2회HCID 866984786-chloro-N-methyl-4-phenylpyridazin-3-amine

생성물 1

HCID 71766225HCID 71766225, 화합물수율 20%

시약·촉매·용매 1

HCID 21899848Ethylacetate heptane용매

실험 절차

The title compound was prepared in analogy to example 1, from (6-chloro-4-phenyl-pyridazin-3-yl)-methyl-amine and 3-methanesulfonyl-5-trifluoromethyl-benzoic acid (example 1, intermediate d) after a reaction time of 18 hours and using a gradient of n-heptane:ethyl acetate (100:0 to 30:70) for the chromatographic purification. Another purification step using preparative HPLC (Gemini NX column) with a gradient of methanol:water with 0.05% formic acid (80:20 to 98:2) gave the desired compound as a colorless solid (20%). MS (ESI+): m/z=470.054 ([M+H]+).

후처리

  1. customfor the chromatographic purification
  2. customAnother purification step

출처 및 근거

ORD 기록
ord-e7337ea0e16c4a81881f3913ad10d58d
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748434B2

반응 노트

불러오는 중…