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Sodium Hydroxide → 4-[N-(3-Cyano-4-neopentyloxyphenyl)carbamoyl]-3-methylpyrazol-1-ylacetic acid

HRID 1744580
ノート
印刷プレビュー

反応式

HRID 1744580 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([NH:15][C:16]([C:18]2[C:19]([CH3:29])=[N:20][N:21]([CH2:23][C:24]([O:26]CC)=[O:25])[CH:22]=2)=[O:17])[CH:6]=[CH:7][C:8]=1[O:9][CH2:10][C:11]([CH3:14])([CH3:13])[CH3:12])#[N:2].[OH-].[Na+]>C(O)C>[C:1]([C:3]1[CH:4]=[C:5]([NH:15][C:16]([C:18]2[C:19]([CH3:29])=[N:20][N:21]([CH2:23][C:24]([OH:26])=[O:25])[CH:22]=2)=[O:17])[CH:6]=[CH:7][C:8]=1[O:9][CH2:10][C:11]([CH3:14])([CH3:13])[CH3:12])#[N:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 22228013Ethyl 4-[N-(3-cyano-4-neopentyloxyphenyl)carbamoyl]-3-methylpyrazol-1-ylacetate

生成物 1

HCID 222282094-[N-(3-Cyano-4-neopentyloxyphenyl)carbamoyl]-3-methylpyrazol-1-ylacetic acid収率 30.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethyl 4-[N-(3-cyano-4-neopentyloxyphenyl)carbamoyl]-3-methylpyrazol-1-ylacetate (0.7 g) was added to ethanol (5 ml) and 10% aqueous sodium hydroxide solution (5 ml) was added. The mixture was stirred at a refluxing temperature for 30 min. The solvent was evaporated under reduced pressure. To the residue was added dilute hydrochloric acid and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. Diisopropyl ether was added to the residue to allow crystallization. The crystals were recrystallized from a mixed solvent of ethyl acetate-diisopropyl ether to give the title compound (0.2 g), melting point: 234–245° C.

後処理

  1. additionwas added
  2. customThe solvent was evaporated under reduced pressure
  3. additionTo the residue was added dilute hydrochloric acid
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customafter which the solvent was evaporated under reduced pressure
  8. additionDiisopropyl ether was added to the residue
  9. customcrystallization
  10. customThe crystals were recrystallized from a mixed solvent of ethyl acetate-diisopropyl ether

出典と根拠

ORDレコード
ord-45712526133a4423a9e7690273262fbb
出典データセット
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07015218B1

反応ノート

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