4-Methylmorpholine → HCID 178508425, 화합물

HRID 2173714노트

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HRID 2173714 반응식
[NH2:1][C:2]1[C:3]([C:13]([OH:15])=O)=[N:4][C:5]([Br:12])=[C:6]([C:8]([F:11])([F:10])[F:9])[N:7]=1.[NH:16]1[C:20]2=[N:21][CH:22]=[CH:23][N:24]=[C:19]2[C:18]([NH2:25])=[N:17]1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CN1CCOCC1>CN(C=O)C.O>[NH2:1][C:2]1[C:3]([C:13]([NH:25][C:18]2[C:19]3=[N:24][CH:23]=[CH:22][N:21]=[C:20]3[NH:16][N:17]=2)=[O:15])=[N:4][C:5]([Br:12])=[C:6]([C:8]([F:9])([F:10])[F:11])[N:7]=1

참가 물질

7

반응물 4

HCID 79724-MethylmorpholineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 584422963-Amino-6-bromo-5-trifluoromethyl-pyrazine-2-carboxylic acid2회HCID 178509233HCID 178509233, 화합물

생성물 1

HCID 178508425HCID 178508425, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture comprising 3-amino-6-bromo-5-trifluoromethyl-pyrazine-2-carboxylic acid (Intermediate 2)(0.212 g, 0.740 mmol), 1H-pyrazolo[3,4-b]pyrazin-3-amine (0.10 g, 0.740 mmol), HATU (0.281 g, 0.740 mmol) and N-methylmorpholine (0.146 ml, 1.480 mmol) in DMF (5 ml) was stirred at RT for 45 minutes. The reaction mixture was diluted with water (25 ml) and the resulting orange precipitate was filtered under vacuum and washed with water (10 ml). The solid was purified by chromatography on silica, eluting with iso-hexane:EtOAc (gradient of 0 to 100% EtOAc) to afford the title compound as a yellow solid.

후처리

  1. filtrationthe resulting orange precipitate was filtered under vacuum
  2. washwashed with water (10 ml)
  3. customThe solid was purified by chromatography on silica
  4. washeluting with iso-hexane

출처 및 근거

ORD 기록
ord-c27425cf65d04451a66fc94e7f525ca4
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09056867B2

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