3-Nitrosalicylic acid → 2-Benzyloxy-3-nitro-benzoic Acid Benzyl Ester

HRID 1064840노트

반응식

HRID 1064840 반응식
C(=O)([O-])[O-].[K+].[K+].[N+:7]([C:10]1[CH:18]=[CH:17][CH:16]=[C:12]([C:13]([OH:15])=[O:14])[C:11]=1[OH:19])([O-:9])=[O:8].[CH2:20](Br)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>CN(C=O)C.O>[CH2:20]([O:19][C:11]1[C:10]([N+:7]([O-:9])=[O:8])=[CH:18][CH:17]=[CH:16][C:12]=1[C:13]([O:15][CH2:13][C:12]1[CH:16]=[CH:17][CH:18]=[CH:10][CH:11]=1)=[O:14])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

참가 물질

6

반응물 3

HCID 68073-Nitrosalicylic acidHCID 7498Benzyl BromideHCID 11430Potassium Carbonate

생성물 1

HCID 161066762-Benzyloxy-3-nitro-benzoic Acid Benzyl Ester수율 162.3%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

Potassium carbonate (16.6 g, 120.1 mmol) was added to a solution of 3-nitrosalicylic acid (10 g, 54.6 mmol) in DMF (100 ml) and benzyl bromide (14.3 ml, 120.1 mmol) was dropped thereinto. The mixture was stirred at 80° C. for 12 hours and the reaction solution was diluted with water and extracted with ether. The organic layer was washed with water and a saturated sodium chloride solution successively, dried over anhydrous sodium sulfate and the solvent was evaporated therefrom to provide 16.1 g (yield 81%) of benzyl 2-benzyloxy-3-nitrobenzoate as brown oil.

후처리

  1. additionwas dropped
  2. extractionextracted with ether
  3. washThe organic layer was washed with water
  4. dry with materiala saturated sodium chloride solution successively, dried over anhydrous sodium sulfate
  5. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-76696d917e2a459a86cc68998cf3ba90
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06969711B2

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