Methyl 2-(bis((tert-butoxy)carbonyl)amino)prop-2-enoate → 2-(Di-tert-butoxycarbonylamino)-3-(7,7-dimethyl-1,4,6,7-tetrahydro-pyrazolo[4,3-c]pyridin-5-yl)-propionic acid methyl ester

HRID 2250212

반응식

HRID 2250212 반응식
[CH3:1][C:2]1([CH3:11])[CH2:7][NH:6][CH2:5][C:4]2[CH:8]=[N:9][NH:10][C:3]1=2.[CH3:12][O:13][C:14](=[O:32])[C:15]([N:17]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=[CH2:16]>CO>[CH3:12][O:13][C:14](=[O:32])[CH:15]([N:17]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[C:18]([O:20][C:21]([CH3:24])([CH3:22])[CH3:23])=[O:19])[CH2:16][N:6]1[CH2:7][C:2]([CH3:11])([CH3:1])[C:3]2[NH:10][N:9]=[CH:8][C:4]=2[CH2:5]1

참가 물질

4

반응물 2

HCID 10870342Methyl 2-(bis((tert-butoxy)carbonyl)amino)prop-2-enoateHCID 211022097,7-dimethyl-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine

생성물 1

HCID 588644042-(Di-tert-butoxycarbonylamino)-3-(7,7-dimethyl-1,4,6,7-tetrahydro-pyrazolo[4,3-c]pyridin-5-yl)-propionic acid methyl ester

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 7,7-dimethyl-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine (160 mg) in methanol (3 mL) was added 2-(di-tert-butoxycarbonylamino)-acrylic acid methyl ester (331 mg). A gentle stream of nitrogen was applied and the reaction stirred overnight. In the morning, the volume was greatly reduced. The last traces of solvent were removed under high vacuum to give 490 mg (quant.) which was used without purification. 1H-NMR (CDCl3, 500 MHz) δ 1.24 (s, 3H), 1.26 (s, 3H), 1.38 (s, 18H), 2.33 (d, J=11.3, 1H), 2.57 (d, J=11.3, 1H), 3.09 (dd, J=13.1, 5.5, 1H), 3.15 (dd, J=13.4, 9.5, 1H), 3.35 (d, J=12.8, 1H), 3.57 (d, J=12.8, 1H), 3.68 (s, 3H), 5.13 (dd, J=9.5, 3.7, 1H), 7.16 (s, 1H). Mass spec.: 453.30 (MH)+.

후처리

  1. customThe last traces of solvent were removed under high vacuum
  2. customto give 490 mg (quant.) which
  3. customwas used without purification

출처 및 근거

ORD 기록
ord-cbfc953eef1c4710900b76d32331a38b
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07314883B2

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