Methyl iodide → HCID 67076777、化合物

HRID 521515ノート

反応式

HRID 521515 の反応式
[CH2:1]([O:3][C:4](=[O:25])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][CH2:13][C:14]2[CH:15]=[C:16]([CH3:20])[CH:17]=[CH:18][CH:19]=2)=[C:7]([O:21][C:22](=O)C)[CH:6]=1)C.CC(C)([O-])C.[K+].C(=O)([O-])[O-].[K+].[K+].IC>CO>[CH3:1][O:3][C:4](=[O:25])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][CH2:13][C:14]2[CH:15]=[C:16]([CH3:20])[CH:17]=[CH:18][CH:19]=2)=[C:7]([O:21][CH3:22])[CH:6]=1

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 23665647Potassium tert-butoxideHCID 670767713-Acetoxy-4-(2-m-tolyl-ethoxy)-benzoic acid ethyl ester

生成物 1

HCID 67076777HCID 67076777、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The compound of step 2 (150 mg, 0.438 mmol) was dissolved in methanol (3 ml), potassium tert-butoxide (73 mg, 0.657 mmol) was added and the mixture was stirred overnight under reflux. Potassium carbonate (60 mg, 0.44 mmol) and iodomethane (124 mg, 0.876 mmol) were then added repeatedly, at intervals of 1 h, with stirring under reflux until completion of the reaction. The volatiles were evaporated in vacuo, the residue was partitioned between EA and 2 N hydrochloric acid, and the aqueous phase was extracted with EA. The combined organic phases were dried over sodium chloride, decanted and evaporated to dryness to yield the title compound.

後処理

  1. temperatureunder reflux
  2. stirringwith stirring
  3. temperatureunder reflux until completion of the reaction
  4. customThe volatiles were evaporated in vacuo
  5. customthe residue was partitioned between EA and 2 N hydrochloric acid
  6. extractionthe aqueous phase was extracted with EA
  7. dry with materialThe combined organic phases were dried over sodium chloride
  8. customdecanted
  9. customevaporated to dryness

出典と根拠

ORDレコード
ord-e7050a94cfd74d45a83000b5a166f66a
出典データセット
uspto-grants-2016_05
特許番号
US09328071B2

反応ノート

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