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Potassium Carbonate → (5-Chloro-2,3-dihydrobenzofuran-2-yl)methanol

HRID 1772243
ノート
印刷プレビュー

反応式

HRID 1772243 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([CH2:9][CH:10]=[CH2:11])[CH:3]=1.C1C=C(Cl)C=C(C(OO)=[O:20])C=1.C(=O)([O-])[O-].[K+].[K+]>C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]2[O:8][CH:10]([CH2:11][OH:20])[CH2:9][C:4]=2[CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 841432-Allyl-4-chlorophenol

生成物 1

HCID 23244655(5-Chloro-2,3-dihydrobenzofuran-2-yl)methanol

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
50 °C

実験手順

To a solution of 4-chloro-2-(prop-2-en-1-yl)phenol (17 g, crude, nominally 101 mmol) in chloroform (100 ml) was added mCPBA (17.4 g, 101 mmol, 1 eq) with stirring for 1 h at 50° C. in an oil bath. Then the reaction mixture was concentrated under vacuum and re-dissolved in MeOH (100 ml). Potassium carbonate (27.6 g, 200 mmol, 2 eq) was added and the mixture was stirred for 5 hours at 50° C. The solids were filtered off and the filtrate was concentrated under vacuum. The crude material was purified by silica gel chromatography using 3% ethyl acetate in petroleum ether to elute. The product-containing fractions were combined and concentrated under vacuum to afford (5-chloro-2,3-dihydro-1-benzofuran-2-yl)methanol as yellow oil (6.15 g); 1H NMR (300 MHz, CDCl3): δ 7.00-7.18 (m, 2H), 6.80 (d, J=8.7 Hz, 1H), 4.88-4.97 (m, 1H), 3.85-3.90 (m, 1H), 3.70-3.79 (m, 1H), 3.19-3.27 (dd, J=9.3 Hz, 15.9 Hz, 1H), 2.98-3.05 (dd, J=7.5 Hz, 15.9 Hz, 1H), 2.10 (broad s, 1H).

後処理

  1. concentrationThen the reaction mixture was concentrated under vacuum
  2. dissolutionre-dissolved in MeOH (100 ml)
  3. stirringthe mixture was stirred for 5 hours at 50° C
  4. filtrationThe solids were filtered off
  5. concentrationthe filtrate was concentrated under vacuum
  6. customThe crude material was purified by silica gel chromatography
  7. washto elute
  8. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-c5fd025394a84d038e438962e14a0072
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09249102B2

反応ノート

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