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2-Aminooxazole → 5(S)-Oxazol-2-ylaminomethyl-3-(3-fluoro-4-(3,6-dihydro-(2H)-pyran-4-yl)phenyl)oxazolidin-2-one

HRID 1582368
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HRID 1582368 반응식
[NH2:1][C:2]1[O:3][CH:4]=[CH:5][N:6]=1.[Li]CCCC.CS(O[CH2:17][C@@H:18]1[O:22][C:21](=[O:23])[N:20]([C:24]2[CH:29]=[CH:28][C:27]([C:30]3[CH2:31][CH2:32][O:33][CH2:34][CH:35]=3)=[C:26]([F:36])[CH:25]=2)[CH2:19]1)(=O)=O>C1COCC1>[O:3]1[CH:4]=[CH:5][N:6]=[C:2]1[NH:1][CH2:17][C@@H:18]1[O:22][C:21](=[O:23])[N:20]([C:24]2[CH:29]=[CH:28][C:27]([C:30]3[CH2:31][CH2:32][O:33][CH2:34][CH:35]=3)=[C:26]([F:36])[CH:25]=2)[CH2:19]1
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참가 물질

5

반응물 3

HCID 5585212-AminooxazoleHCID 213566765(R)-methanesulfonyloxymethyl 3-(4-[3,6-dihydro-(2H)-pyran-4-yl]-3-fluorophenyl)oxazolidin-2-oneHCID 178418339Butyllithium

생성물 1

HCID 207257125(S)-Oxazol-2-ylaminomethyl-3-(3-fluoro-4-(3,6-dihydro-(2H)-pyran-4-yl)phenyl)oxazolidin-2-one수율 4.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매
2회

실험 절차

To a stirred partial solution of 2-aminooxazole(169 mg, 2.0 mmol) in dry THF (10 ml), cooled to −78° C., under argon, was added slowly n-BuLi(1.33M, 1.5 ml, 2.0 mmol), followed after 1 h by 5(R)-methylsulfonyloxymethyl-3-(3-fluoro-4-(3,6-dihydro-(2H)-pyran-4-yl)phenyl)oxazolidin-2-one (see Example 41; 371 mg, 1.0 mol) suspended in dry THF(20 ml). The reaction was allowed to come to room temperature and then refluxed for 24 h. The reaction was quenched with ammonium chloride solution(10%w/v, 30 ml), extracting the mixture with chloroform (3×50 ml). The extracts were dried (magnesium sulfate), concentrated by rotary evaporation chromatographed by MPLC (Merck 9385 silica, 3-10% gradient methanol/dichloromethane eluent) and the pure fractions combined, concentrated and triturated with diethyl ether to. give the title compound (25 mg, 4.6%). NMR (300 Mz, DMSO-d6), δ/ppm: 2.31 (m, 2H), 3.35 (m, 2H, obscured), 3.64 (dd, 1H), 3.84 (t, 2H), 3.90 (m, 1H), 4.15 (m, 1H), 4.24 (m, 2H), 4.46 (m, 1H), 5.97 (m, 1H), 6.90 (m, 1H), 7.19 (m, 2H, partially obscured), 7.37 (dd, 1H), 7.44 (dd, 1H). MS: ES+ (M+H)=360.

후처리

  1. customto come to room temperature
  2. temperaturerefluxed for 24 h
  3. customThe reaction was quenched with ammonium chloride solution(10%w/v, 30 ml),
  4. extractionextracting the mixture with chloroform (3×50 ml)
  5. dry with materialThe extracts were dried (magnesium sulfate)
  6. concentrationconcentrated by rotary evaporation
  7. customchromatographed by MPLC (Merck 9385 silica, 3-10% gradient methanol/dichloromethane eluent)
  8. concentrationconcentrated
  9. customtriturated with diethyl ether to

출처 및 근거

ORD 기록
ord-9c4c17896ab8406392af38a7a5bd9ace
출처 데이터셋
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06734200B1

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