Pyridine, 2-[(trimethylsilyl)oxy]- → HCID 67884043, 화합물

HRID 1613602노트

반응식

HRID 1613602 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

HCID 67884043HCID 67884043, 화합물

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-37455526beb64936be4509d373808791
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194442

반응 노트

불러오는 중…