4-Methylmorpholine → HCID 178451528, 화합물

HRID 2173715노트

반응식

HRID 2173715 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.[NH2:16][C:17]1[NH:21][N:20]=[C:19]2[CH2:22][N:23]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:24][C:18]=12.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:16][C:17]2[NH:21][N:20]=[C:19]3[CH2:22][N:23]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:24][C:18]=23)=[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 178451527HCID 178451527, 화합물

생성물 1

HCID 178451528HCID 178451528, 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)(0.102 g, 0.357 mmol), tert-butyl 3-amino-4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate (0.08 g, 0.357 mmol), HATU (0.136 g, 0.357 mmol) and N-methylmorpholine (0.071 ml, 0.713 mmol) in DMF (5 ml) was stirred at RT for 30 minutes. The reaction mixture was diluted with water (15 ml) and the resulting orange precipitate was filtered under vacuum and washed with water (10 ml). Purification of the resulting solid by chromatography on silica eluting with iso-hexane:EtOAc (gradient of 0 to 100% EtOAc) to afforded the title compound as a yellow solid.

후처리

  1. filtrationthe resulting orange precipitate was filtered under vacuum
  2. washwashed with water (10 ml)
  3. customPurification of the resulting solid by chromatography on silica eluting with iso-hexane

출처 및 근거

ORD 기록
ord-458b9a33df4e433b89e2743c2ffcc2f4
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09056867B2

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