Methanol → HCID 15062404、化合物

HRID 486849ノート

反応式

HRID 486849 の反応式
CC1(C)O[C:6](=[O:8])[CH:5]=[C:4]([CH2:9][CH:10]([OH:13])[CH2:11][Cl:12])[O:3]1.C(=O)([O-])[O-].[K+].[K+].CO>C(OCC)(=O)C>[Cl:12][CH2:11][CH:10]1[O:13][C:6](=[O:8])[CH2:5][C:4](=[O:3])[CH2:9]1

参加物

5

反応物 3

HCID 887Methanol2 回HCID 11430Potassium CarbonateHCID 14944829HCID 14944829、化合物

生成物 1

HCID 15062404HCID 15062404、化合物収率 74%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 940 mg (4.26 mmol) of (-)-2,2-dimethyl-6-(3-chloro-2-hydroxypropyl)-1,3-dioxin-4-one (98% ee), 882 mg (6.39 mmol) of potassium carbonate and 10 ml of methanol was stirred at room temperature for 12 hours. After completion of the reaction, methanol was distilled off, and the resultant residue was neutralized with 10% HCl and then extracted with ethyl acetate, followed by drying over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was subjected to column chromatography (an eluent of hexane:ethyl acetate=3:1), thereby obtaining 510 mg (yield 74%) of (-)-6-chloromethyltetrahydropyran-2,4-dione.

後処理

  1. distillationwas distilled off
  2. extractionextracted with ethyl acetate
  3. dry with materialby drying over anhydrous magnesium sulfate
  4. distillationAfter the solvent was distilled off

出典と根拠

ORDレコード
ord-118aa606c6fb42efbeefd59031e5a285
出典データセット
uspto-grants-1994_03
特許番号
US05292891

反応ノート

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