Nitric Acid → Ethyl 3-(4-nitrobenzyl)cyclobutanecarboxylate

HRID 1713857노트

반응식

HRID 1713857 반응식
[N+:1]([O-:4])(O)=[O:2].S(=O)(=O)(O)O.[CH2:10]([CH:17]1[CH2:20][CH:19]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH2:18]1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(Cl)Cl>[N+](C1C=CC=CC=1)([O-])=O>[N+:1]([C:14]1[CH:15]=[CH:16][C:11]([CH2:10][CH:17]2[CH2:20][CH:19]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH2:18]2)=[CH:12][CH:13]=1)([O-:4])=[O:2]

참가 물질

6

반응물 4

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 6344DichloromethaneHCID 20313172Ethyl 3-benzylcyclobutanecarboxylate

생성물 1

HCID 59464076Ethyl 3-(4-nitrobenzyl)cyclobutanecarboxylate

시약·촉매·용매 1

HCID 7416Nitrobenzene용매

실험 절차

A mixture of concentrated nitric acid (0.5 mL) and concentrated sulphuric acid (0.8 mL) was added slowly with stirring to an ice-cooled solution of ethyl 3-benzylcyclobutanecarboxylate (German Patent DE 2626287) (876 mmol, 4.02 mmol) in nitrobenzene (2 mL). The reaction mixture was warmed to ambient temperature and stirred for 1.5 h then poured onto ice/water. DCM (5 mL) was added and the mixture was stirred before passing through a phase separation cartridge. Solvent was removed by evaporation to give the title compound that was used directly in the next step.

후처리

  1. additionwas added slowly
  2. additionthen poured onto ice/water
  3. stirringthe mixture was stirred
  4. custombefore passing through a phase separation cartridge
  5. customSolvent was removed by evaporation

출처 및 근거

ORD 기록
ord-7fe7a60faf6743ef8546762ca605ea63
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07795283B2

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