Ethanol → Ethyl 4-benzylamino-2-ethoxy-5-nitro-benzoate

HRID 578056노트

반응식

HRID 578056 반응식
[CH2:1]([NH:8][C:9]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:11](F)[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:24]([OH:26])[CH3:25].OS([O-])(=O)=O.[K+]>O>[CH2:1]([NH:8][C:9]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:11]([O:26][CH2:24][CH3:25])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 702Ethanol2회HCID 516920Potassium bisulfateHCID 67230873Ethyl 4-benzylamino-2-fluoro-5-nitro-benzoate

생성물 1

HCID 67233615Ethyl 4-benzylamino-2-ethoxy-5-nitro-benzoate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

The product obtained at (655b) (15.5 g, 2.97 mmol) was combined with a mixture of potassium tert.-butylate (6.00 g, 53.5 mmol) and 400 mL ethanol, that was stirred at ambient temperature already for 15 min. After stirring for 1 h, 400 mL ethanol were added. After further 1 h of stirring, potassium tert.-butylate (500 mg, 4.46 mmol) was added. After further 1.5 h, the mixture was poured into water and acidified with KHSO4 (aq). After stirring for 20 min, the precipitate was filtered off, washed with water and dried at 55° C.

후처리

  1. stirringAfter stirring for 1 h
  2. stirringAfter further 1 h of stirring
  3. waitAfter further 1.5 h
  4. stirringAfter stirring for 20 min
  5. filtrationthe precipitate was filtered off
  6. washwashed with water
  7. customdried at 55° C.

출처 및 근거

ORD 기록
ord-df6e1412688b4290a9c3ca04481397d0
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040565B2

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