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

HRID 657964

反応式

HRID 657964 の反応式
[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]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 581368013-tert-butyl-N-methoxy-5-(2-methoxyethoxy)-N-methylbenzamideHCID 178418573HCID 178418573、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-82c79826129b4f49a7366ce680b36a0a
出典データセット
uspto-grants-2011_12
特許番号
US08076336B2

関連ノート

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