Water → HCID 12769820、化合物

HRID 26687

反応式

HRID 26687 の反応式
[CH2:1]([CH:3]1[CH:8]([CH3:9])[C:7](=[O:10])[C:6]2[CH:11]=[C:12]([CH:15]([CH3:20])[C:16]([O:18]C)=[O:17])[CH:13]=[CH:14][C:5]=2[O:4]1)[CH3:2].C(=O)(O)[O-].[Na+].O>C(O)C>[CH2:1]([CH:3]1[CH:8]([CH3:9])[C:7](=[O:10])[C:6]2[CH:11]=[C:12]([CH:15]([CH3:20])[C:16]([OH:18])=[O:17])[CH:13]=[CH:14][C:5]=2[O:4]1)[CH3:2]

参加物

5

反応物 3

HCID 962WaterHCID 516892Sodium BicarbonateHCID 21322013Methyl 2-[2,3-dihydro-2-ethyl-3-methyl-4-oxo-4H-1-benzopyran-6-yl]propionate

生成物 1

HCID 12769820HCID 12769820、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Methyl 2-[2,3-dihydro-2-ethyl-3-methyl-4-oxo-4H-1-benzopyran-6-yl]propionate (6 g) was dissolved in ethanol (200 ml) and heated to reflux with dilute aqueous sodium bicarbonate solution (50 ml) for eight hours. The reaction mixture was poured into water, acidified and extracted with ether. The combined etheral extracts were washed with water and dried (MgSO4) and concentrated in vacuo affording a mixture of the desired product and starting material which were separated by chromatography on silica gel using dichloromethane/ether mixtures as eluant. The title compound was recrystallised from petroleum ether (bp 40°-60° C.) as a white solid: 1.4 g, mp 114°-115° C.

後処理

  1. temperatureheated
  2. extractionextracted with ether
  3. washThe combined etheral extracts were washed with water
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customaffording

出典と根拠

ORDレコード
ord-c6d54deac7e142829d3b2da97761ea92
出典データセット
uspto-grants-1979_04
特許番号
US04151179

関連ノート

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