Diisopropylethylamine → Tert-butyl 3-[(6-amino-5-nitropyridin-2-yl)amino]piperidine-1-carboxylate

HRID 57694

반응식

HRID 57694 반응식
[NH2:1][CH:2]1[CH2:7][CH2:6][CH2:5][N:4]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:3]1.[NH2:15][C:16]1[C:21]([N+:22]([O-:24])=[O:23])=[CH:20][CH:19]=[C:18](Cl)[N:17]=1.C(N(C(C)C)CC)(C)C>CS(C)=O>[NH2:15][C:16]1[N:17]=[C:18]([NH:1][CH:2]2[CH2:7][CH2:6][CH2:5][N:4]([C:8]([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9])[CH2:3]2)[CH:19]=[CH:20][C:21]=1[N+:22]([O-:24])=[O:23]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 5458091-BOC-3-AminopiperidineHCID 27240356-Chloro-3-nitropyridin-2-ylamine

생성물 1

HCID 57911762Tert-butyl 3-[(6-amino-5-nitropyridin-2-yl)amino]piperidine-1-carboxylate

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
120 °C

실험 절차

500 mg (2.11 mmol) of tert-butyl 3-aminopiperidine-1-carboxylate, 772 mg (4.22 mmol) of 2-amino-6-chloro-3-nitropyridine and 1.05 ml (6.34 mmol) of diisopropylethylamine were suspended in 18 ml of DMSO and heated in a microwave reactor at 120° C. for 45 min. The reaction mixture was purified by preparative reverse-phase HPLC. This gave 600 mg (81% of theory) of the product as a solid.

후처리

  1. customThe reaction mixture was purified by preparative reverse-phase HPLC

출처 및 근거

ORD 기록
ord-168e6acda84543759bf4d6b4fd981bc9
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434731B2

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