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

HRID 1053787ノート

反応式

HRID 1053787 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-cc51561050704db3ba33c61cfc045b75
出典データセット
uspto-grants-2016_07
特許番号
US09394273B2

反応ノート

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