Hydrochloric Acid → N-(1,6-dichloro-2-naphthyl)carbamic acid ethyl ester

HRID 1270772노트

반응식

HRID 1270772 반응식
[CH2:1]([O:3][C:4](=[O:17])[NH:5][C:6]1[CH:15]=[CH:14][C:13]2[C:8](=[CH:9][CH:10]=[C:11]([Cl:16])[CH:12]=2)[CH:7]=1)[CH3:2].[Cl:18]N1C(=O)CCC1=O.Cl.O>C(O)(=O)C>[CH2:1]([O:3][C:4](=[O:17])[NH:5][C:6]1[CH:15]=[CH:14][C:13]2[C:8](=[CH:9][CH:10]=[C:11]([Cl:16])[CH:12]=2)[C:7]=1[Cl:18])[CH3:2]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 31398ChlorosuccinimideHCID 68803058N-(6-chloro-2-naphthyl)carbamic acid ethyl ester

생성물 1

HCID 68803921N-(1,6-dichloro-2-naphthyl)carbamic acid ethyl ester

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

반응 조건

온도
50 °C

실험 절차

A mixture of N-(6-chloro-2-naphthyl)carbamic acid ethyl ester (725 mg, 2.90 mmol), N-chlorosuccinimide (387 mg, 2.90 mmol) and 1 M HCl in acetic acid (2.90 mL, 2.90 mmol) in acetic acid (20 mL) is heated at 50° C. under N2 atmosphere for 1 hour. After cooling to room temperature, water (10 mL) is added and extracted with EtOAc. The organic layer is washed with brine, dried (Na2SO4) and concentrated by rotary evaporator to give N-(1,6-dichloro-2-naphthyl)carbamic acid ethyl ester as a yellow solid.

후처리

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with EtOAc
  3. washThe organic layer is washed with brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated by rotary evaporator

출처 및 근거

ORD 기록
ord-172da2645f774c2ab22370424b1158b9
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07202364B2

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