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

HRID 224388노트

반응식

HRID 224388 반응식
[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

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 21226445Aluminium lithium hydrideHCID 23332965HCID 23332965, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cb836e190bc84a4ebd3aa1b1f8198efb
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04232032

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