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Nitric Acid → HCID 20094336、化合物

HRID 273843
ノート
印刷プレビュー

反応式

HRID 273843 の反応式
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([CH2:13][CH:14]([Br:16])[CH3:15])=[CH:10][CH:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[N+:17]([O-])([OH:19])=[O:18]>C(O)(=O)C>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([CH2:13][CH:14]([Br:16])[CH3:15])=[CH:10][C:11]=2[N+:17]([O-:19])=[O:18])[CH2:6][CH2:5]1)(=[O:3])[CH3:2]
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 944Nitric AcidHCID 200943701-Acetyl-5-(2-bromopropyl)indoline

生成物 1

HCID 20094336HCID 20094336、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a solution of 1-acetyl-5-(2-bromopropyl)indoline (153 g) in acetic acid (240 ml) was added fuming nitric acid (120 ml) with stirring under ice cooling over a period of 1 hour, and the mixture was stirred at room temperature for 30 minutes. After the reaction mixture was poured into ice water slowly, the precipitates were collected by filtration, and dissolved in benzene (1.5 l). The benzene solution was washed with water, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was recrystallized from ethyl acetate-isopropyl ether to give 155 g of 1-acetyl-5-(2-bromopropyl)-7-nitroindoline melting at 119°-120° C.

後処理

  1. stirringthe mixture was stirred at room temperature for 30 minutes
  2. filtrationthe precipitates were collected by filtration
  3. dissolutiondissolved in benzene (1.5 l)
  4. washThe benzene solution was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue was recrystallized from ethyl acetate-isopropyl ether

出典と根拠

ORDレコード
ord-eac9aa3827ec4723b1d6eec944f571c8
出典データセット
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05387603

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート