Hydrogen Bromide → 2-Bromo-1-(2,3-dihydro-1,4-benzodioxin-2-yl)ethan-1-ol

HRID 225145노트

반응식

HRID 225145 반응식
[Br:1][CH2:2][C:3]([CH:5]1[O:10][C:9]2[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=2[O:7][CH2:6]1)=[O:4].[BH4-].[Na+].Br>CO>[O:10]1[C:9]2[CH:11]=[CH:12][CH:13]=[CH:14][C:8]=2[O:7][CH2:6][CH:5]1[CH:3]([OH:4])[CH2:2][Br:1]

참가 물질

5

반응물 3

HCID 260Hydrogen BromideHCID 4311764Sodium borohydrideHCID 126085852-Bromo-1-(2,3-dihydro-1,4-benzodioxin-2-yl)ethan-1-one

생성물 1

HCID 126085902-Bromo-1-(2,3-dihydro-1,4-benzodioxin-2-yl)ethan-1-ol수율 25.8%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
-70 °C

실험 절차

2-Bromoacetyl-1,4-benzodioxan(53.8 g) in methanol (500 mls) was cooled to -70° C. Sodium borohydride (10.3 g) was added and the solution stirred at -70° C. for 12 hours. The solution was treated with hydrobromic acid until acidic and the solvent evaporated. The residue was dissolved in ether and the ether extracts were washed with sodium bicarbonate solution; then water and dried (MgSO4) and evaporated to give a white solid. This was recrystallised eight times from petroleum spirit 60-80 to give 14 grams of the title compound.

후처리

  1. customevaporated
  2. dissolutionThe residue was dissolved in ether
  3. washthe ether extracts were washed with sodium bicarbonate solution
  4. dry with materialthen water and dried (MgSO4)
  5. customevaporated
  6. customto give a white solid
  7. customThis was recrystallised eight times from petroleum spirit 60-80

출처 및 근거

ORD 기록
ord-49ade3456d8649a7ba63b43f907aac16
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04235915

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