Methyl iodide → HCID 67076777, 화합물

HRID 521515노트

반응식

HRID 521515 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 67076777HCID 67076777, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e7050a94cfd74d45a83000b5a166f66a
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09328071B2

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