Triethylamine → HCID 86686015, 화합물

HRID 2277720노트

반응식

HRID 2277720 반응식
[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]

참가 물질

7

반응물 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, 화합물

생성물 1

HCID 86686015HCID 86686015, 화합물수율 45.5%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-12f4882d4bf840209f944c390ae18522
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133158B2

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