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

HRID 578056ノート

反応式

HRID 578056 の反応式
[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

参加物

5

反応物 3

HCID 702Ethanol2 回HCID 516920Potassium bisulfateHCID 67230873Ethyl 4-benzylamino-2-fluoro-5-nitro-benzoate

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-df6e1412688b4290a9c3ca04481397d0
出典データセット
uspto-grants-2015_05
特許番号
US09040565B2

反応ノート

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