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Sodium Hydroxide → HCID 58488523、化合物

HRID 451367
ノート
印刷プレビュー

反応式

HRID 451367 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[NH:13][CH:12]=[C:11]([C:14]([O:16]C)=[O:15])[C:10]=1[CH3:18].[OH-].[Na+]>CO>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[NH:13][CH:12]=[C:11]([C:14]([OH:16])=[O:15])[C:10]=1[CH3:18]
参加物反応条件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 58488518methyl 5-(2-chloro-4-fluorophenyl)-4-methyl-1H-pyrrole-3-carboxylate

生成物 1

HCID 58488523HCID 58488523、化合物収率 100.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
80 °C

実験手順

To a solution of methyl 5-(2-chloro-4-fluorophenyl)-4-methyl-1H-pyrrole-3-carboxylate (0.64 g, 2.4 mmol) in methanol (10 ml) was added 5N NaOH (10 ml) and the mixture was stirred at 80° C. for 4.0 h. The reaction mixture was concentrated on a rotary evaporator. To the residue was added water and washed with Et2O. The resulting solution was neutralized with conc HCl and extracted with ethyl acetate. The organic layer was washed with water and brine, then dried over sodium sulfate and concentrated on a rotary evaporator to give the title compound (610 mg, quant) as a brown solid.

後処理

  1. concentrationThe reaction mixture was concentrated on a rotary evaporator
  2. additionTo the residue was added water
  3. washwashed with Et2O
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with water and brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated on a rotary evaporator

出典と根拠

ORDレコード
ord-c1c84ca280644972b23e69b4f3753b2c
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08487117B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート