Hydrochloric Acid → 1-[3-Tert-butyl-5-(2-methoxyethoxy)phenyl]ethanone

HRID 532380

반응식

HRID 532380 반응식
[C:1]([C:5]1[CH:6]=[C:7]([CH:14]=[C:15]([O:17][CH2:18][CH2:19][O:20][CH3:21])[CH:16]=1)[C:8](N(OC)C)=[O:9])([CH3:4])([CH3:3])[CH3:2].[CH3:22][Mg]Br.Cl>C1COCC1.O>[C:1]([C:5]1[CH:6]=[C:7]([C:8](=[O:9])[CH3:22])[CH:14]=[C:15]([O:17][CH2:18][CH2:19][O:20][CH3:21])[CH:16]=1)([CH3:2])([CH3:3])[CH3:4]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 581368013-tert-butyl-N-methoxy-5-(2-methoxyethoxy)-N-methylbenzamideHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 581368081-[3-Tert-butyl-5-(2-methoxyethoxy)phenyl]ethanone

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

3-tert-Butyl-N-methoxy-5-(2-methoxyethoxy)-N-methylbenzamide (O3.043; 1.35 g) was dissolved in THF (40 ml), methylmagnesium bromide (3.05 ml, 3 M in ether) was added dropwise at 0° C. and then the mixture was stirred at RT for 2 h. Then the mixture was admixed with 1 N hydrochloric acid (50 ml), diluted with water and extracted by shaking three times with EA. Then the combined EA phases were dried over magnesium sulfate, filtered and concentrated. The residue was purified using silica gel (40 g cartridge, n-heptane/EA gradient of 0-30% in 30 min). 1.0 g of the title compound were obtained.

후처리

  1. extractionextracted
  2. stirringby shaking three times with EA
  3. dry with materialThen the combined EA phases were dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified
  7. customsilica gel (40 g cartridge, n-heptane/EA gradient of 0-30% in 30 min)

출처 및 근거

ORD 기록
ord-51cdb4316a464836ac5a55e7e965462a
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08853206B2

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