Sodium Hydroxide → 7-(4-Tert-butylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid

HRID 566004ノート

反応式

HRID 566004 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]=[CH:13][C:14]3[O:20][CH2:19][CH2:18][C:17]([C:21]([O:23]CC)=[O:22])=[CH:16][C:15]=3[CH:26]=2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Na+]>C(O)C>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([C:11]2[CH:12]=[CH:13][C:14]3[O:20][CH2:19][CH2:18][C:17]([C:21]([OH:23])=[O:22])=[CH:16][C:15]=3[CH:26]=2)=[CH:9][CH:10]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 18472239Ethyl 7-(4-tert-butylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylate

生成物 1

HCID 184722187-(4-Tert-butylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid収率 85.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of ethyl 7-(4-tert-butylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylate (503.8 mg) in ethanol (10 ml)was added 1N sodium hydroxide (2.0 m) at room temperature, and the mixture was stirred for 64 hours and concentrated under reduced pressure. To the residue was added 1N hydrochloric acid (15 ml), and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride solution, dried with magnesium sulfate and concentrated. The resulting crystal was collected by filtration to give 7-(4-tert-butylphenyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid (396 mg) as colorless crystals.

後処理

  1. concentrationconcentrated under reduced pressure
  2. additionTo the residue was added 1N hydrochloric acid (15 ml)
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated sodium chloride solution
  5. dry with materialdried with magnesium sulfate
  6. concentrationconcentrated
  7. filtrationThe resulting crystal was collected by filtration

出典と根拠

ORDレコード
ord-7eb64510c37d4f589387182df96a37ec
出典データセット
uspto-grants-2001_01
特許番号
US06172061B2

反応ノート

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