Ethanol → HCID 59515926, 화합물

HRID 1161288노트

반응식

HRID 1161288 반응식
[C:1]([O:4][CH2:5][CH2:6][NH:7][C:8]1[C:9]([N+:25]([O-])=O)=[C:10]2[C:15](=[CH:16][CH:17]=1)[C:14](=[O:18])[N:13]([CH2:19][CH2:20][O:21][C:22](=[O:24])[CH3:23])[CH:12]=[CH:11]2)(=[O:3])[CH3:2].C(O)C.[Cl-].[NH4+].O>[Fe].C(Cl)Cl>[C:1]([O:4][CH2:5][CH2:6][NH:7][C:8]1[C:9]([NH2:25])=[C:10]2[C:15](=[CH:16][CH:17]=1)[C:14](=[O:18])[N:13]([CH2:19][CH2:20][O:21][C:22](=[O:24])[CH3:23])[CH:12]=[CH:11]2)(=[O:3])[CH3:2]

참가 물질

7

반응물 4

HCID 702EthanolHCID 962WaterHCID 25517Ammonium ChlorideHCID 595159322-(2-(2-Acetoxyethyl)-5-nitro-1-oxo-1,2-dihydroisoquinolin-6-ylamino)ethyl acetate

생성물 1

HCID 59515926HCID 59515926, 화합물

시약·촉매·용매 2

HCID 23925Iron촉매HCID 6344Dichloromethane용매

실험 절차

A mixture of 2-(2-(2-acetoxyethyl)-5-nitro-1-oxo-1,2-dihydroisoquinolin-6-ylamino)ethyl acetate (350 mg, 0.00093 mol), ethanol (20 mL, 0.3 mol), ammonium chloride (496.1 mg, 0.009275 mol) and water (10 mL, 0.6 mol) was added at 85° C. Iron (207 mg, 0.00371 mol) was added in two portions five minutes apart and the reaction was stirred at that temperature for 1 hour. The reaction mixture was then poured into methylene chloride (100 mL) and the layers were separated and the organic layer was washed with brine and dried over sodium sulfate. The solvent was removed under reduced pressure and used for the next reaction without purification. MS m/z=348.5 (M+H).

후처리

  1. additionwas added at 85° C
  2. customthe layers were separated
  3. washthe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customused for the next reaction without purification

출처 및 근거

ORD 기록
ord-eb025335bb97488d810a1b8adc44b24e
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07816371B2

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