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Potassium Hydroxide → 1H-Pyrrole, 3-(phenylmethyl)-

HRID 1156495
ノート
印刷プレビュー

反応式

HRID 1156495 の反応式
[C:1]([C:9]1[CH:10]=[C:11](C(OC)=O)[NH:12][CH:13]=1)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[K+].O.NN>C(O)COCCOCCO>[CH2:1]([C:9]1[CH:10]=[CH:11][NH:12][CH:13]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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

5

反応物 3

HCID 14797Potassium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 2764013Methyl 4-benzoyl-1H-pyrrole-2-carboxylate

生成物 1

HCID 117688281H-Pyrrole, 3-(phenylmethyl)-収率 71.2%

試薬・触媒・溶媒 1

HCID 8172Triethylene Glycol溶媒

反応条件

温度
120 °C

実験手順

12.0 g (52.4 mmole) of methyl 4-benzoyl-2-pyrrolecarboxylate, 8.79 g (157 mmole) of potassium hydroxide and 10.5 g (210 mmole) of hydrazine hydrate are dissolved in 150 ml of triethylene glycol. Reaction is carried out by stirring the solution at 120° C. for 2 hours and then at 160° C. for 3 hours in the an atmosphere of nitrogen gas. After reaction is finished, the reaction solution is allowed to cool and poured into ice water, followed by extraction with ether. The extract is washed with water saturated with sodium chloride and concentrated. The residue is distilled under reduced pressure to obtain 5.86 g of 3-benzylpyrrole as a colorless liquid. Yield 71.2%. nD29.5 1.5790. Boiling point 95°-98° C. (0.09 mmHg).

後処理

  1. customReaction
  2. waitat 160° C. for 3 hours in the an atmosphere of nitrogen gas
  3. customAfter reaction
  4. temperatureto cool
  5. extractionfollowed by extraction with ether
  6. washThe extract is washed with water saturated with sodium chloride
  7. concentrationconcentrated
  8. distillationThe residue is distilled under reduced pressure

出典と根拠

ORDレコード
ord-cd5eaf82df5545a6a7a410f4be75f15c
出典データセット
uspto-grants-1982_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04336194

反応ノート

読み込み中…

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