4-Methylmorpholine → HCID 178508425、化合物

HRID 2173714ノート

反応式

HRID 2173714 の反応式
[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

参加物

7

反応物 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 acid2 回HCID 178509233HCID 178509233、化合物

生成物 1

HCID 178508425HCID 178508425、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c27425cf65d04451a66fc94e7f525ca4
出典データセット
uspto-grants-2015_06
特許番号
US09056867B2

反応ノート

読み込み中…