Water → 2-(2,3-Dihydro-1,4-benzodioxin-6-yl)ethan-1-ol

HRID 1053787노트

반응식

HRID 1053787 반응식
B.C1COCC1.[O:7]1[CH2:12][CH2:11][O:10][C:9]2[CH:13]=[C:14]([CH2:17][C:18](O)=[O:19])[CH:15]=[CH:16][C:8]1=2.O>C1COCC1>[O:7]1[CH2:12][CH2:11][O:10][C:9]2[CH:13]=[C:14]([CH2:17][CH2:18][OH:19])[CH:15]=[CH:16][C:8]1=2

참가 물질

5

반응물 3

HCID 962WaterHCID 870201,4-Benzodioxan-6-ylacetic acidHCID 2723981Borane;tetrahydrofuran

생성물 1

HCID 197468082-(2,3-Dihydro-1,4-benzodioxin-6-yl)ethan-1-ol수율 99%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

BH3.THF (44 mL, 44 mmol, 1 M/THF) was added to a 0° C. solution of 2-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)acetic acid (3.419 g, 17.6 mmol) in THF (8.8 mL). The reaction was allowed to warm to room temperature and after 2 h, 20 mL H2O was added slowly by syringe. The resulting mixture was extracted with ethyl acetate, the organic portion was washed with brine, and then was dried (Na2SO4), filtered and evaporated. Purification by flash chromatography (ethyl acetate/hexanes) gave the title compound (3.059 g, 99%).

후처리

  1. extractionThe resulting mixture was extracted with ethyl acetate
  2. washthe organic portion was washed with brine
  3. dry with materialwas dried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated
  6. customPurification by flash chromatography (ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-cc51561050704db3ba33c61cfc045b75
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394273B2

반응 노트

불러오는 중…