4-Methylmorpholine → ((S)-1-{[(3,5-Diamino-6-chloro-pyrazine-2-carbonyl)-amino]-methyl}-butyl)-carbamic acid tert-butyl ester

HRID 1183021노트

반응식

HRID 1183021 반응식
[C:1]([O:5][C:6](=[O:14])[NH:7][C@H:8]([CH2:12][NH2:13])[CH2:9][CH2:10][CH3:11])([CH3:4])([CH3:3])[CH3:2].[NH2:15][C:16]1[C:17]([C:24](O)=[O:25])=[N:18][C:19]([Cl:23])=[C:20]([NH2:22])[N:21]=1.CN1CCOCC1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C>[C:1]([O:5][C:6](=[O:14])[NH:7][C@H:8]([CH2:12][NH:13][C:24]([C:17]1[C:16]([NH2:15])=[N:21][C:20]([NH2:22])=[C:19]([Cl:23])[N:18]=1)=[O:25])[CH2:9][CH2:10][CH3:11])([CH3:2])([CH3:3])[CH3:4]

참가 물질

6

반응물 4

HCID 79724-MethylmorpholineHCID 64521193,5-Diamino-6-chloro-pyrazine acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 86651886((S)-1-Aminomethyl-butyl)-carbamic acid tert-butyl ester

생성물 1

HCID 86651887((S)-1-{[(3,5-Diamino-6-chloro-pyrazine-2-carbonyl)-amino]-methyl}-butyl)-carbamic acid tert-butyl ester

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of ((S)-1-aminomethyl-butyl)-carbamic acid tert-butyl ester (1.70 g, 8.40 mmol), 3,5-diamino-6-chloro-pyrazine-2-carboxylic acid (1.59 g, 8.43 mmol), N-methylmorpholine (3.8 mL, 34.5 mmol) and HATU (3.2 g, 8.42 mmol) in anhydrous DMF (50 mL) is stirred at RT for 16 h. The reaction mixture is concentrated in vacuo and the resulting residue is purified by column chromatography (basic alumina, MeOH:DCM) to afford the title compound as yellow solid. [M+H]+ 333.

후처리

  1. concentrationThe reaction mixture is concentrated in vacuo
  2. customthe resulting residue is purified by column chromatography (basic alumina, MeOH:DCM)

출처 및 근거

ORD 기록
ord-0cccc2e793234150be418124d328a5fa
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08664228B2

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