Sodium Hydroxide → 11-Hydroxy-11-methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic Acid

HRID 894217ノート

反応式

HRID 894217 の反応式
[OH:1][C:2]1([CH3:21])[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17]([O:19]C)=[O:18])=[CH:16][C:3]1=2.[OH-].[Na+]>C(O)C>[OH:1][C:2]1([CH3:21])[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17]([OH:19])=[O:18])=[CH:16][C:3]1=2

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 21162722Methyl 11-hydroxy-11-methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate

生成物 1

HCID 1292913211-Hydroxy-11-methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic Acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Dissolve 450 mg. of methyl 11-hydroxy-11-methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate in 20 ml. of ethanol and add 20 ml. of 5% aqueous sodium hydroxide solution. Stir at room temperature for 1 hour. Evaporate the alcohol and dilute the residual sodium salt solution with 40 ml of water. Cool in an ice bath and acidify with 5N hydrochloric acid. Separate the solids by filtration and dry (yield 250 mg). Recrystallize from benzene to obtain the title product (yield 200 mg., m.p. 258°-258° C.).

後処理

  1. dissolutionDissolve 450 mg
  2. customEvaporate the alcohol
  3. additiondilute the residual sodium salt solution with 40 ml of water
  4. temperatureCool in an ice bath
  5. customSeparate the solids
  6. filtrationby filtration
  7. customdry (yield 250 mg)
  8. customRecrystallize from benzene

出典と根拠

ORDレコード
ord-f8f3a18c970e4f9bbcacf8918a22c125
出典データセット
uspto-grants-1981_08
特許番号
US04282365

反応ノート

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