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Acetic Acid → HCID 11283696、化合物

HRID 915287
ノート
印刷プレビュー

反応式

HRID 915287 の反応式
Cl[CH:2]([O:4][C:5](=[O:32])[N:6]([C:29](=[O:31])[CH3:30])[CH2:7][C@@H:8]1[O:12][C:11](=[O:13])[N:10]([C:14]2[CH:19]=[CH:18][C:17]([CH:20]3[CH2:25][CH2:24][S:23](=[O:27])(=[O:26])[CH2:22][CH2:21]3)=[C:16]([F:28])[CH:15]=2)[CH2:9]1)[CH3:3].[C:33]([OH:36])(=[O:35])[CH3:34].CCOCC>C([O-])(=O)C.[Hg+2].C([O-])(=O)C.O>[C:29]([N:6]([CH2:7][C@@H:8]1[O:12][C:11](=[O:13])[N:10]([C:14]2[CH:19]=[CH:18][C:17]([CH:20]3[CH2:25][CH2:24][S:23](=[O:27])(=[O:26])[CH2:22][CH2:21]3)=[C:16]([F:28])[CH:15]=2)[CH2:9]1)[C:5]([O:4][CH:2]([O:36][C:33](=[O:35])[CH3:34])[CH3:3])=[O:32])(=[O:31])[CH3:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 176Acetic AcidHCID 3283Diethyl EtherHCID 58958558HCID 58958558、化合物

生成物 1

HCID 11283696HCID 11283696、化合物収率 43%

試薬・触媒・溶媒 2

HCID 15337Mercuric acetate触媒HCID 962Water溶媒

実験手順

Acetyl-{3-[4-(1,1-dioxo-hexahydro-1λ6-thiopyran-4-yl)-3-fluoro-phenyl]-2-oxo-oxazolidin 5(R)-ylmethyl}-carbamic acid 1(R,S)-chloro-ethyl ester (11) (0.49 g, 1 mmol), mercury(II) acetate (0.37 g, 1.175 mmol), and acetic acid (6.3 mL, 109 mmol) are stirred at RT overnight. Ether and water are added and the layers are separated. The organic layer is washed several times with water, brine, dried over Na2SO4 and conc in vacuo. After purification by silica gel chromatography, the product is re-dissolved in CH2Cl2 and washed with several portions of sat NaHCO3, water, dried over Na2SO4 and conc in vacuo to give the title compound in 43% yield (0.51 g) as a mixture of two diastereomers in a 1:1 ratio. 1H NMR (400 MHz, CDCl3): δ 7.46 (dt, 1H), 7.21 (m, 1H), 7.13 (m, 1H), 6.88 (q, 1H), 4.82 (m, 0.5H), 4.75 (m, 0.5H), 4.13 (m, 1H), 4.04 (m, 2H), 3.73 (dd, 0.5H), 3.67 (dd, 0.5H), 3.12 (m, 5H), 2.55 (s, 1.5H), 2.53 (s, 1.5H), 2.38 (m, 2H), 2.17 (m, 2H), 2.13 (s, 1.5H), 2.06 (s, 1.5H), 1.57 (d, 1.5H), 1.54 (d, 1.5H). MS-APCI (m/z+): 341, 385, 427, 515.

後処理

  1. customthe layers are separated
  2. washThe organic layer is washed several times with water, brine
  3. dry with materialdried over Na2SO4 and conc in vacuo
  4. customAfter purification by silica gel chromatography
  5. dissolutionthe product is re-dissolved in CH2Cl2
  6. washwashed with several portions of sat NaHCO3, water
  7. dry with materialdried over Na2SO4 and conc in vacuo

出典と根拠

ORDレコード
ord-b22a746944d24f00b1f1b32f4cebadf0
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07265140B2

反応ノート

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