Trifluoroacetic acid → HCID 58739080, 화합물

HRID 720293노트

반응식

HRID 720293 반응식
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]([N:22]2[CH2:27][CH2:26][CH:25]([OH:28])[CH2:24][CH2:23]2)[N:9]([CH3:21])[C:10](=[O:20])[C:11]=1[O:12]CC1C=CC=CC=1)=[O:5])[CH3:2].[F:29][C:30]([F:35])([F:34])[C:31](O)=[O:32]>>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]([N:22]2[CH2:27][CH2:26][CH:25]([O:28][C:31](=[O:32])[C:30]([F:35])([F:34])[F:29])[CH2:24][CH2:23]2)[N:9]([CH3:21])[C:10](=[O:20])[C:11]=1[OH:12])=[O:5])[CH3:2]

참가 물질

3

반응물 2

HCID 6422Trifluoroacetic acidHCID 21060062HCID 21060062, 화합물

생성물 1

HCID 58739080HCID 58739080, 화합물

실험 절차

5-Benzyloxy-2-(4-hydroxypiperidin-1-yl)-1-methyl-6-oxo-1,6-dihydropyrimidine-4-carboxylic acid ethyl ester (0.760 g, 1.96 mmol) was treated with trifluroacetic acid (20 mL) at ambient temperature. After 10 h, the reaction mixture was concentrated and purified on silica gel column using 2–5% MeOH/CH2Cl2 to afford desired product as a brown paste (0.650 g, 84%). 1H NMR (500 MHz, CDCl3) δ: 10.02 (br s, 1H), 5.23–5.19 (m, 1H), 4.44 (q, J=7.0 Hz, 2H), 3.57 (s, 3H), 3.36–3.31 (m, 2H), 3.15–3.10 (m, 2H), 2.17–2.11 (m, 2H), 2.02–1.95 (m, 2H), 1.42 (t, J=7.0 Hz, 3H). LRMS (M+H) calcd for C15H19F3N3O6: 394.32. found: 394.09

후처리

  1. concentrationthe reaction mixture was concentrated
  2. custompurified on silica gel column

출처 및 근거

ORD 기록
ord-60b9a6b894e4486d9f6a88b5ba3dcfb5
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07135467B2

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