Carbonic acid, bis(1,1-dimethylethyl) ester → Tert-butyl 4-((6-aminopyridin-2-yl)methyl)piperazine-1-carboxylate

HRID 520485노트

반응식

HRID 520485 반응식
[N:1]1([CH2:7][C:8]2[N:13]=[C:12]([NH2:14])[CH:11]=[CH:10][CH:9]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:15](=O)([O:21]C(C)(C)C)[O:16][C:17]([CH3:20])([CH3:19])[CH3:18]>C1COCC1.CN(C)C1C=CN=CC=1>[NH2:14][C:12]1[N:13]=[C:8]([CH2:7][N:1]2[CH2:6][CH2:5][N:4]([C:15]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:21])[CH2:3][CH2:2]2)[CH:9]=[CH:10][CH:11]=1

참가 물질

5

반응물 2

HCID 10219638Carbonic acid, bis(1,1-dimethylethyl) esterHCID 585528446-(Piperazin-1-ylmethyl)picolinonitrile

생성물 1

HCID 58552896Tert-butyl 4-((6-aminopyridin-2-yl)methyl)piperazine-1-carboxylate

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 6-(piperazin-1-ylmethyl)pyridin-2-amine 85 in THF was added di-tert-butyl carbonate (1 eq) and 4-(dimethyl)aminopyridine (catalytic). The reaction mixture was stirred at room temperature for 18 h. It was then concentrated under reduced pressure. Pentane was added and the resulting solid was collected by filtration and dried to afford 86. The Boc protecting group could be removed after coupling with the appropriate carboxylic acid by treatment with TFA/CH2Cl2 for 12 h.

후처리

  1. concentrationIt was then concentrated under reduced pressure
  2. additionPentane was added
  3. filtrationthe resulting solid was collected by filtration
  4. customdried

출처 및 근거

ORD 기록
ord-5882411819754903bf2a6cd903d258c2
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09326986B2

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