Methyl 2-t-butoxycarbonylamino-4-[4-[4-(4-pyridyl)-piperazin-1-yl]phenoxy]butyrat → Methyl 2-amino-4-[4-[4-(4-pyridyl)piperazin-1-yl]-phenoxy]butyrate

HRID 2249노트

반응식

HRID 2249 반응식
C(OC([NH:8][CH:9]([CH2:14][CH2:15][O:16][C:17]1[CH:22]=[CH:21][C:20]([N:23]2[CH2:28][CH2:27][N:26]([C:29]3[CH:34]=[CH:33][N:32]=[CH:31][CH:30]=3)[CH2:25][CH2:24]2)=[CH:19][CH:18]=1)[C:10]([O:12][CH3:13])=[O:11])=O)(C)(C)C>C(O)(C(F)(F)F)=O>[NH2:8][CH:9]([CH2:14][CH2:15][O:16][C:17]1[CH:18]=[CH:19][C:20]([N:23]2[CH2:24][CH2:25][N:26]([C:29]3[CH:34]=[CH:33][N:32]=[CH:31][CH:30]=3)[CH2:27][CH2:28]2)=[CH:21][CH:22]=1)[C:10]([O:12][CH3:13])=[O:11]

참가 물질

3

반응물 1

HCID 18918622Methyl 2-t-butoxycarbonylamino-4-[4-[4-(4-pyridyl)-piperazin-1-yl]phenoxy]butyrat

생성물 1

HCID 18918214Methyl 2-amino-4-[4-[4-(4-pyridyl)piperazin-1-yl]-phenoxy]butyrate수율 74.1%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

The compound of Example 140 (0.96 g) in TFA (10 ml) was kept at room temperature for 2 hours. The solution was evaporated and the residue dissolved in water (15 ml) and the solution basified with sodium carbonate. The mixture was extracted three times with dichloromethane. Evaporation of the combined extracts gave the title compound (0.56 g); m.p. 125°-127° C.; NMR(d6DMSO) δ 8.2(2H,d), 6.92(6H,m), 4.0(2H,m), 3.64(3H,s), 3.46(4H,t), 3.15(4H,t), 2.04(2H,m), 1.84(1H, m); m/e 371(M+H)+. Calculated for C20H26N4 O3. 0.75 H2O: C, 62.5; H, 7.17; N, 14.6. Found: C, 62.8; H, 6.8; N, 14.3%.

후처리

  1. customThe solution was evaporated
  2. dissolutionthe residue dissolved in water (15 ml)
  3. extractionThe mixture was extracted three times with dichloromethane
  4. customEvaporation of the combined extracts

출처 및 근거

ORD 기록
ord-bc4c5bfd0a2540ebba7d4dbbdd3411b3
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728701

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