Triethylamine → HCID 86686015、化合物

HRID 2277720ノート

反応式

HRID 2277720 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[N:6]([C:12]1[CH:13]=[N:14][CH:15]=[C:16]([N:18]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)[CH:17]=1)[C:5]2([CH3:25])[CH3:24].[Cl:26][C:27]1[C:28]([C:33](O)=[O:34])=[N:29][CH:30]=[CH:31][CH:32]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(CC)CC>C(Cl)Cl.O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[N:6]([C:12]1[CH:13]=[N:14][CH:15]=[C:16]([N:18]3[CH2:23][CH2:22][N:21]([C:33]([C:28]4[C:27]([Cl:26])=[CH:32][CH:31]=[CH:30][N:29]=4)=[O:34])[CH2:20][CH2:19]3)[CH:17]=1)[C:5]2([CH3:25])[CH3:24]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 8246323-Chloropyridine-2-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 86686012HCID 86686012、化合物

生成物 1

HCID 86686015HCID 86686015、化合物収率 45.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of 5-chloro-3,3-dimethyl-2-(5-piperazin-1-yl-pyridin-3-yl)-2,3-dihydro-isoindol-1-one (example 455 [C]) (52 mg, 0.146 mmol), 3-chloro-pyridine-2-carboxylic acid (25.3 mg, 0.161 mmol), HATU (83.3 mg, 0.219 mmol) and Et3N (29.5 mg, 0.292 mmol) in DCM (5 mL) was stirred for 2 hours at room temperature. The mixture was treated with water, and extracted with DCM. The organic layer was dried over anhy. Na2SO4 and after removal of solvent, the residue was purified by preparative HPLC to afford the title compound (33 mg, 45%) as a white solid. MS: 496.3 (M+H+).

後処理

  1. extractionextracted with DCM
  2. customThe organic layer was dried over anhy
  3. customNa2SO4 and after removal of solvent
  4. customthe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-12f4882d4bf840209f944c390ae18522
出典データセット
uspto-grants-2015_09
特許番号
US09133158B2

反応ノート

読み込み中…