Diisopropylethylamine → Tert-butyl 3-(tert-butyldimethylsilyloxy)-5-((7-chloropyrido[4,3-b]pyrazin-5-ylamino)methyl)piperidine-1-carboxylate

HRID 57537노트

반응식

HRID 57537 반응식
[NH2:1][CH2:2][CH:3]1[CH2:8][CH:7]([O:9][Si:10]([C:13]([CH3:16])([CH3:15])[CH3:14])([CH3:12])[CH3:11])[CH2:6][N:5]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:4]1.Cl[C:25]1[C:34]2[C:29](=[N:30][CH:31]=[CH:32][N:33]=2)[CH:28]=[C:27]([Cl:35])[N:26]=1.CCN(C(C)C)C(C)C>C1COCC1>[Si:10]([O:9][CH:7]1[CH2:8][CH:3]([CH2:2][NH:1][C:25]2[C:34]3[C:29](=[N:30][CH:31]=[CH:32][N:33]=3)[CH:28]=[C:27]([Cl:35])[N:26]=2)[CH2:4][N:5]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:6]1)([C:13]([CH3:16])([CH3:15])[CH3:14])([CH3:12])[CH3:11]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 71113882Tert-butyl 3-(aminomethyl)-5-(tert-butyldimethylsilyloxy)piperidine-1-carboxylateHCID 717428275,7-Dichloropyrido(3,4-b)pyrazine

생성물 1

HCID 86717367Tert-butyl 3-(tert-butyldimethylsilyloxy)-5-((7-chloropyrido[4,3-b]pyrazin-5-ylamino)methyl)piperidine-1-carboxylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of tert-butyl 3-(aminomethyl)-5-(tert-butyldimethylsilyloxy)piperidine-1-carboxylate (4.74 g, 13.7 mmol), 5,7-dichloropyrido[4,3-b]pyrazine (2.75 g, 13.7 mmol) and DIPEA (2.12 g, 16.4 mmol) in THF (20 mL) was stirred at room temperature for 48 hours. The volatiles were removed under reduced pressure and the residue was treated with ethyl acetate, washed with brine, dried over Na2SO4, filtered, and concentrated to give the title compound.

후처리

  1. customThe volatiles were removed under reduced pressure
  2. additionthe residue was treated with ethyl acetate
  3. washwashed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ae9081071dd44d79a66c0acbafdd85e9
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434726B2

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