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HCID 58458920, 화합물 → HCID 136224431, 화합물

HRID 390359
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HRID 390359 반응식
C([O:8][C:9]1[C:18](=[O:19])[N:17]2[C:12]([C:13]([CH3:21])([CH3:20])[O:14][CH2:15][CH2:16]2)=[N:11][C:10]=1[C:22]1[O:23][C:24]([CH2:27][C:28]2[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=2)=[N:25][N:26]=1)C1C=CC=CC=1>C(O)(C(F)(F)F)=O>[F:34][C:31]1[CH:32]=[CH:33][C:28]([CH2:27][C:24]2[O:23][C:22]([C:10]3[N:11]=[C:12]4[N:17]([C:18](=[O:19])[C:9]=3[OH:8])[CH2:16][CH2:15][O:14][C:13]4([CH3:21])[CH3:20])=[N:26][N:25]=2)=[CH:29][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 58458920HCID 58458920, 화합물

생성물 1

HCID 136224431HCID 136224431, 화합물수율 62.7%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of 3-(benzyloxy)-2-(5-(4-fluorobenzyl)-1,3,4-oxadiazol-2-yl)-9,9-dimethyl-6,7-dihydropyrimido[2,1-c][1,4]oxazin-4(9H)-one (0.071 g, 0.15 mmol) in TFA (5 mL) was stirred 22 h at room temperature. The reaction mixture was then concentrated and purified by preparative HPLC on a C18 column using water/MeOH containing 0.1% TFA as eluent to afford the title compound (0.035 g, 60% yield) as white solid. 1HNMR (500 MHz, CDCl3) δ: 9.71 (1H, s), 7.35 (2H, dd, J=8.6, 5.5 Hz), 7.06 (2H, t, J=8.6 Hz), 4.30 (2H, s), 4.07-4.03 (4H, m), 1.63 (6H, s). HRMS (M+H) calcd for C18H18N4O4F: 373.1312. found: 373.1326. Anal calcd for C18H17N4O4F: C, 58.06; H, 4.60; N, 15.04. found: C, 57.88; H, 4.72; N, 14.87.

후처리

  1. concentrationThe reaction mixture was then concentrated
  2. custompurified by preparative HPLC on a C18 column

출처 및 근거

ORD 기록
ord-f45876bbb62a4ebe94f40ecf6fc1e0de
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08383639B2

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