Tetrabutylammonium Fluoride Trihydrate → HCID 67884017, 화합물

HRID 1613599노트

반응식

HRID 1613599 반응식
O.O.O.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[O:22]1[CH:29]2[CH:23]1[CH2:24][CH2:25][O:26][C:27]1[CH:33]=[CH:32][CH:31]=[CH:30][C:28]=12.[Cl:34][C:35]1[CH:36]=[CH:37][C:38]([O:41][Si](C)(C)C)=[N:39][CH:40]=1>O>[Cl:34][C:35]1[CH:36]=[CH:37][C:38](=[O:41])[N:39]([C@@H:29]2[C:28]3[CH:30]=[CH:31][CH:32]=[CH:33][C:27]=3[O:26][CH2:25][CH2:24][C@H:23]2[OH:22])[CH:40]=1

참가 물질

5

반응물 3

HCID 11726816Tetrabutylammonium Fluoride TrihydrateHCID 13149080HCID 13149080, 화합물HCID 14517467HCID 14517467, 화합물

생성물 1

HCID 67884017HCID 67884017, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

22.7 g (72 mmol) of tetrabutylammonium fluoride trihydrate are added to a mixture of 10.54 g (65 mmol) of 4,5-epoxy-2,3,4,5-tetrahydro-1-benzoxepin and 19.4 g (96 mmol) of 5-chloro-2-trimethylsilyloxy-pyridine, and the mixture is heated at 90° C. for 3 hours. The mixture is stirred into water and extracted several times with ethyl acetate. The combined organic phases are washed with water and saturated sodium chloride solution, and the solvent is evaporated off in vacuo. The residue is crystallized in n-butyl acetate. Crystals of melting point 175.5°-177.5° C. are obtained.

후처리

  1. extractionextracted several times with ethyl acetate
  2. washThe combined organic phases are washed with water and saturated sodium chloride solution
  3. customthe solvent is evaporated off in vacuo
  4. customThe residue is crystallized in n-butyl acetate
  5. customCrystals of melting point 175.5°-177.5° C. are obtained

출처 및 근거

ORD 기록
ord-3cad651ae9ba4f6ab02a8b651151dfe6
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194442

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