Tetrabutylammonium Fluoride Trihydrate → HCID 67884017、化合物

HRID 1613599ノート

反応式

HRID 1613599 の反応式
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

参加物

5

反応物 3

HCID 11726816Tetrabutylammonium Fluoride TrihydrateHCID 13149080HCID 13149080、化合物HCID 14517467HCID 14517467、化合物

生成物 1

HCID 67884017HCID 67884017、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3cad651ae9ba4f6ab02a8b651151dfe6
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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