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Nitric Acid → HCID 20094336, 화합물

HRID 273843
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HRID 273843 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 200943701-Acetyl-5-(2-bromopropyl)indoline

생성물 1

HCID 20094336HCID 20094336, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-eac9aa3827ec4723b1d6eec944f571c8
출처 데이터셋
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05387603

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