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2-Chloromethyl-2-(2-fluoro-4-trifluoromethylphenyl)oxirane → 2-(2-Fluoro-4-trifluoromethylphenyl)-2-(1,2,4-triazol-1-ylmethyl)oxirane

HRID 1732152
ノート
印刷プレビュー

反応式

HRID 1732152 の反応式
Cl[CH2:2][C:3]1([C:6]2[CH:11]=[CH:10][C:9]([C:12]([F:15])([F:14])[F:13])=[CH:8][C:7]=2[F:16])[CH2:5][O:4]1.[NH:17]1[CH:21]=[N:20][CH:19]=[N:18]1.[Na]>C(O)(C)(C)C>[F:16][C:7]1[CH:8]=[C:9]([C:12]([F:15])([F:14])[F:13])[CH:10]=[CH:11][C:6]=1[C:3]1([CH2:2][N:17]2[CH:21]=[N:20][CH:19]=[N:18]2)[CH2:5][O:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 202267062-Chloromethyl-2-(2-fluoro-4-trifluoromethylphenyl)oxiraneHCID 454898221h-1,2,4-Triazole sodium salt

生成物 1

HCID 202266732-(2-Fluoro-4-trifluoromethylphenyl)-2-(1,2,4-triazol-1-ylmethyl)oxirane

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

A solution of 2-chloromethyl-2-(2-fluoro-4-trifluoromethylphenyl)oxirane (6 g.) in tert-butyl alcohol was treated with sodium 1,2,4-triazole (2.7 g.) and heated at 100° for 1 hour. The mixture was evaporated and the residual gum partitioned between ethyl acetate and water. the organic layer was washed with water, dried and evaporated to dryness. The residual gum was chromatographed on K60 silica gel using chloroform/petroleum ether (b.p. 60°-80°) 1:1 v/v and chloroform as eluting solvents to give 2-(2-fluoro-4-trifluoromethylphenyl)-2-(1,2,4-triazol-1-ylmethyl)oxirane, as a gum with NMR data as follows:

後処理

  1. temperatureheated at 100° for 1 hour
  2. customThe mixture was evaporated
  3. customthe residual gum partitioned between ethyl acetate and water
  4. washthe organic layer was washed with water
  5. customdried
  6. customevaporated to dryness
  7. customThe residual gum was chromatographed on K60 silica gel
  8. washas eluting solvents

出典と根拠

ORDレコード
ord-738947c28531464abb32b4ecf161b996
出典データセット
uspto-grants-1986_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04625036

反応ノート

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