Methylamine → 3-(1-(isopropylamino)phthalazin-6-yl)-N,4-dimethylbenzamide

HRID 2357537ノート

反応式

HRID 2357537 の反応式
[CH:1]([NH:4][C:5]1[C:14]2[C:9](=[CH:10][C:11]([C:15]3[CH:16]=[C:17]([CH:21]=[CH:22][C:23]=3[CH3:24])[C:18]([OH:20])=O)=[CH:12][CH:13]=2)[CH:8]=[N:7][N:6]=1)([CH3:3])[CH3:2].CN.[CH3:27][N:28](C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.C(Cl)Cl>[CH:1]([NH:4][C:5]1[C:14]2[C:9](=[CH:10][C:11]([C:15]3[CH:16]=[C:17]([CH:21]=[CH:22][C:23]=3[CH3:24])[C:18]([NH:28][CH3:27])=[O:20])=[CH:12][CH:13]=2)[CH:8]=[N:7][N:6]=1)([CH3:3])[CH3:2]

参加物

6

反応物 3

HCID 6329MethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 684556533-(1-(Isopropylamino)phthalazin-6-yl)-4-methylbenzoic acid

生成物 1

HCID 684548743-(1-(isopropylamino)phthalazin-6-yl)-N,4-dimethylbenzamide

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

A solution of 3-(1-(isopropylamino)phthalazin-6-yl)-4-methylbenzoic acid (0.22 g, 0.7 mmol) in DMF (2 mL) at RT was treated with a 2 M solution of methylamine (2 mL, 3 mmol), and HATU (0.4 g, 1 mmol). The mixture was stirred at RT for 15 h. The mixture was diluted with 100 mL DCM, washed with 20 mL sat. NaHCO3, dried over anhydrous Na2SO4, concentrated in vacuo and purified by column eluting with 2-3% 2M ammonia MeOH/DCM to give the title compound. MS (ES+): 335 (M+H)+.

後処理

  1. washwashed with 20 mL sat. NaHCO3
  2. dry with materialdried over anhydrous Na2SO4
  3. concentrationconcentrated in vacuo
  4. custompurified by column
  5. washeluting with 2-3% 2M ammonia MeOH/DCM

出典と根拠

ORDレコード
ord-01a9ce46d5954e8f8a8dbce623c73db6
出典データセット
uspto-grants-2010_07
特許番号
US07759337B2

反応ノート

読み込み中…