Sodium Hydroxide → HCID 18472317、化合物

HRID 1388024ノート

反応式

HRID 1388024 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([C:7]2[CH:8]=[CH:9][C:10]3[O:16][CH2:15][CH2:14][C:13]([C:17]([O:19]C)=[O:18])=[CH:12][C:11]=3[CH:21]=2)[S:5][CH:6]=1.[OH-].[Na+]>C1COCC1>[CH3:1][C:2]1[CH:3]=[C:4]([C:7]2[CH:8]=[CH:9][C:10]3[O:16][CH2:15][CH2:14][C:13]([C:17]([OH:19])=[O:18])=[CH:12][C:11]=3[CH:21]=2)[S:5][CH:6]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 18472481HCID 18472481、化合物

生成物 1

HCID 18472317HCID 18472317、化合物収率 79.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

In THF (10 ml) was dissolved methyl 7-(4-methyl-2-thienyl)-2,3-dihydro-1-benzoxepine-4-carboxylate (420 mg), and to the mixture was added 1N sodium hydroxide (8.4 ml). The mixture was stirred at room temperature for 15 hours. Under reduced pressure, the organic solvent was removed, and to the residue was added ethyl acetate. The mixture was extracted with water, and to the aqueous layer was added 6N hydrochloric acid to make the solution pH 4-5, which was extracted with ethyl acetate, washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was removed to give 7-(4-methyl-2-thienyl)-2,3-dihydro-1-benzoxepine-4-carboxylic acid (320 mg).

後処理

  1. customUnder reduced pressure, the organic solvent was removed
  2. additionto the residue was added ethyl acetate
  3. extractionThe mixture was extracted with water
  4. additionto the aqueous layer was added 6N hydrochloric acid
  5. extractionwas extracted with ethyl acetate
  6. washwashed with saturated brine
  7. dry with materialdried with magnesium sulfate
  8. customUnder reduced pressure, the solvent was removed

出典と根拠

ORDレコード
ord-118e36ca167049b491db647d652a5279
出典データセット
uspto-grants-2001_07
特許番号
US06268354B1

反応ノート

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