HCID 11994313, 화합물 → N-{5-[Methoxy(phenyl)acetyl]-1,4,5,6-tetrahydropyrrolo[3,4-c]pyrazol-3-yl}-4-(4-methylpiperazin-1-yl)benzene-1-carboximidic acid

HRID 729242노트

반응식

HRID 729242 반응식
[CH3:1][O:2][C@H:3]([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)[C:4]([N:6]1[CH2:13][C:12]2[C:11]([NH:14][C:15](=[O:29])[C:16]3[CH:21]=[CH:20][C:19]([N:22]4[CH2:27][CH2:26][N:25]([CH3:28])[CH2:24][CH2:23]4)=[CH:18][CH:17]=3)=[N:10][N:9](C(OCC)=O)[C:8]=2[CH2:7]1)=[O:5]>CO.C(N(CC)CC)C>[CH3:1][O:2][C@H:3]([C:35]1[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=1)[C:4]([N:6]1[CH2:13][C:12]2[C:11]([NH:14][C:15](=[O:29])[C:16]3[CH:17]=[CH:18][C:19]([N:22]4[CH2:27][CH2:26][N:25]([CH3:28])[CH2:24][CH2:23]4)=[CH:20][CH:21]=3)=[N:10][NH:9][C:8]=2[CH2:7]1)=[O:5]

참가 물질

4

반응물 1

HCID 11994313HCID 11994313, 화합물

생성물 1

HCID 11442891N-{5-[Methoxy(phenyl)acetyl]-1,4,5,6-tetrahydropyrrolo[3,4-c]pyrazol-3-yl}-4-(4-methylpiperazin-1-yl)benzene-1-carboximidic acid수율 46.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8471Triethylamine용매

실험 절차

A solution of ethyl 5-[(2R)-2-methoxy-2-phenylethanoyl]-3-{[4-(4-methylpiperazin-1-yl)benzoyl]amino}-5,6-dihydropyrrolo[3,4-c]pyrazole-1(4H)-carboxylate (3.94 g, 7.2 mmol) in methanol (MeOH, 130 ml) and triethylamine (Et3N, 13 ml) was stirred at room temperature for 16 hours (some precipitation occurred). The solid was separated and washed with Et2O, to give 1.6 g of the title compound. Solution was evaporated up to few milliliters, and a second fraction of solid product was separated (1.62 g). The two fractions were joined and analyzed by LC-MS (purity around 90% 254 and 220 nM). After chromatographic purification (short silica gel column, DCM/MeOH 45:5) 2.83 g (83%) of the title compound were obtained as a white solid. M.p 289° C.; [M+H]+ 475;

후처리

  1. customsome precipitation
  2. customThe solid was separated
  3. washwashed with Et2O

출처 및 근거

ORD 기록
ord-1b031b364ce04fb6be8dadce67a60bba
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582628B2

반응 노트

불러오는 중…