Pyridine, 2-[(trimethylsilyl)oxy]- → HCID 67884043、化合物

HRID 1613602ノート

反応式

HRID 1613602 の反応式
[OH2:1].O.O.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.Br[C@H:23]1[C@H:29](O)[C:28]2[CH:31]=[C:32]([S:35]([C:37]3[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=3)=[O:36])[CH:33]=[CH:34][C:27]=2[O:26][CH2:25][CH2:24]1.C[Si](C)(C)[O:45][C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][N:47]=1>>[O:45]=[C:46]1[CH:51]=[CH:50][CH:49]=[CH:48][N:47]1[C@@H:29]1[C:28]2[CH:31]=[C:32]([S:35]([C:37]3[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=3)=[O:36])[CH:33]=[CH:34][C:27]=2[O:26][CH2:25][CH2:24][C@H:23]1[OH:1]

参加物

4

反応物 3

HCID 10975862Pyridine, 2-[(trimethylsilyl)oxy]-HCID 11726816Tetrabutylammonium Fluoride TrihydrateHCID 67883795trans-4-Bromo-5-hydroxy-7-phenylsulfinyl-2,3,4,5-tetrahydro-1-benzoxepin

生成物 1

HCID 67884043HCID 67884043、化合物

反応条件

温度
60 °C

実験手順

8.60 g (27.3 mmol) of tetrabutylammonium fluoride trihydrate are added to a mixture of 4.00 g (10.9 mmol) of trans-4-bromo-5-hydroxy-7-phenylsulfinyl-2,3,4,5-tetrahydro-1-benzoxepin and 6.40 g (38.3 mmol) of 2-trimethylsilyloxypyridine, and a mixture is subsequently stirred at 60° C. for 5 hours. The cooled syrupy liquid is poured onto ice-water and extracted several times with ethyl acetate. The combined ethyl acetate extracts are washed with water and saturated sodium chloride solution, dried over sodium sulfate, filtered and evaporated. The foamy residue is crystallized in butyl acetate. White crystals of melting point 181°-184° C. are obtained.

後処理

  1. additionThe cooled syrupy liquid is poured onto ice-water
  2. extractionextracted several times with ethyl acetate
  3. washThe combined ethyl acetate extracts are washed with water and saturated sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customThe foamy residue is crystallized in butyl acetate
  8. customWhite crystals of melting point 181°-184° C. are obtained

出典と根拠

ORDレコード
ord-37455526beb64936be4509d373808791
出典データセット
uspto-grants-1993_03
特許番号
US05194442

反応ノート

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