Acetic Anhydride → N-(4-(3-acetamidopiperidin-1-yl)pyridin-3-yl)-3-amino-6-bromopyrazine-2-carboxamide

HRID 69879노트

반응식

HRID 69879 반응식
[NH2:1][C:2]1[C:3]([C:9]([NH:11][C:12]2[CH:13]=[N:14][CH:15]=[CH:16][C:17]=2[N:18]2[CH2:23][CH2:22][CH2:21][CH:20]([NH2:24])[CH2:19]2)=[O:10])=[N:4][C:5]([Br:8])=[CH:6][N:7]=1.C(N(CC)CC)C.[C:32](OC(=O)C)(=[O:34])[CH3:33]>C(Cl)Cl>[C:32]([NH:24][CH:20]1[CH2:21][CH2:22][CH2:23][N:18]([C:17]2[CH:16]=[CH:15][N:14]=[CH:13][C:12]=2[NH:11][C:9]([C:3]2[C:2]([NH2:1])=[N:7][CH:6]=[C:5]([Br:8])[N:4]=2)=[O:10])[CH2:19]1)(=[O:34])[CH3:33]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 866691783-amino-N-(4-(3-aminopiperidin-1-yl)pyridin-3-yl)-6-bromopyrazine-2-carboxamide

생성물 1

HCID 86669177N-(4-(3-acetamidopiperidin-1-yl)pyridin-3-yl)-3-amino-6-bromopyrazine-2-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To solution of 3-amino-N-(4-(3-aminopiperidin-1-yl)pyridin-3-yl)-6-bromopyrazine-2-carboxamide in CH2Cl2 at a concentration of 0.5 M at room temperature was added triethylamine (3 eq) followed by acetic anhydride (1.2 eq). The reaction was stirred at room temperature for 30 minutes, concentrated, purified by reverse phase HPLC and lyophilized to provide N-(4-(3-acetamidopiperidin-1-yl)pyridin-3-yl)-3-amino-6-bromopyrazine-2-carboxamide, as the TFA salt. LCMS (m/z): 434.1 (MH+).

후처리

  1. concentrationconcentrated
  2. custompurified by reverse phase HPLC

출처 및 근거

ORD 기록
ord-d12a126511da4431bd3d642a19543e7f
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822497B2

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