Water → [2,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxin-6-yl]methanol

HRID 224388ノート

反応式

HRID 224388 の反応式
[Cl:1][C:2]([Cl:23])([Cl:22])[CH:3]1[O:8][CH:7]([C:9]([Cl:12])([Cl:11])[Cl:10])[C:6]2[CH:13]=[C:14]([C:17](OCC)=[O:18])[CH:15]=[CH:16][C:5]=2[O:4]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].C(OCC)(=O)C.O>CCOCC>[OH:18][CH2:17][C:14]1[CH:15]=[CH:16][C:5]2[O:4][CH:3]([C:2]([Cl:1])([Cl:22])[Cl:23])[O:8][CH:7]([C:9]([Cl:12])([Cl:11])[Cl:10])[C:6]=2[CH:13]=1

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 21226445Aluminium lithium hydrideHCID 23332965HCID 23332965、化合物

生成物 1

HCID 23332968[2,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxin-6-yl]methanol

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of ethyl 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-carboxylate (2.0 g.) in anhydrous ether (25 ml.) was added at room temperature during 20 minutes to a suspension of lithium aluminium hydride (0.2 g.) in anhydrous ether (25 ml.). The mixture was stirred for 1 hour, then ethyl acetate (5 ml.) was added, followed by water (10 ml.). The mixture was filtered, and the ether layer of the filtrate was separated. The aqueous phase was extracted with ether (3×10 ml.), the combined extracts were dried, and the solvent was evaporated. The residue was crystallised from ethanol to give 6-hydroxymethyl-2,4-bis(trichloromethyl)benzo[1,3]dioxin, m.p. 134°-136° C.

後処理

  1. filtrationThe mixture was filtered
  2. customthe ether layer of the filtrate was separated
  3. extractionThe aqueous phase was extracted with ether (3×10 ml.)
  4. customthe combined extracts were dried
  5. customthe solvent was evaporated
  6. customThe residue was crystallised from ethanol

出典と根拠

ORDレコード
ord-cb836e190bc84a4ebd3aa1b1f8198efb
出典データセット
uspto-grants-1980_11
特許番号
US04232032

反応ノート

読み込み中…