Ethyl formate → HCID 178520855、化合物

HRID 12569

反応式

HRID 12569 の反応式
C[CH2:2][O-:3].[Na+].C(OCC)=O.[C:10]1([C:16]([CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:17])[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>CCO>[OH:17]/[C:16](/[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)=[C:18](/[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)\[CH:2]=[O:3]

参加物

5

反応物 3

HCID 8025Ethyl formateHCID 99482-PhenylacetophenoneHCID 2723922Sodium ethoxide

生成物 1

HCID 178520855HCID 178520855、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
2.5 °C

実験手順

To a cooled solution of NaOEt (763 mg, 11.21 mmol) in EtOH (100 ml) was added ethyl formate (0.91 ml, 11.21 mmol) dropwise. The resulting mixture is allowed to stand for 3 hours at 0 to 5° C., and then deoxybenzoin (2 g, 10.19 mmol) was added. The mixture was stirred for 2 hours at 0 to 5° C. and then placed in the refrigerator for 4 days. After the mixture was stirred overnight at room temperature, it was poured into ice-water, and acidified, and extracted with CH2Cl2. The organic layer was washed with brine, and dried over MgSO4 anhydride, and concentrated in vacuo. The residue was purified by column chromatography (10% ethyl acetate in hexane) to give the title compound as a light yellow solid.

後処理

  1. waitplaced in the refrigerator for 4 days
  2. stirringAfter the mixture was stirred overnight at room temperature
  3. extractionextracted with CH2Cl2
  4. washThe organic layer was washed with brine
  5. dry with materialdried over MgSO4 anhydride
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by column chromatography (10% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-8e50eceeef0549698f541ac6041518dd
出典データセット
uspto-grants-2010_06
特許番号
US07728014B2

関連ノート

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