Potassium Carbonate → Phenyl 4-methoxy-3-(trifluoromethyl)phenylcarbamate

HRID 631445노트

반응식

HRID 631445 반응식
[CH3:1][O:2][C:3]1[CH:9]=[CH:8][C:6]([NH2:7])=[CH:5][C:4]=1[C:10]([F:13])([F:12])[F:11].C(=O)([O-])[O-].[K+].[K+].Cl[C:21]([O:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)=[O:22]>O1CCCC1>[CH3:1][O:2][C:3]1[CH:9]=[CH:8][C:6]([NH:7][C:21](=[O:22])[O:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[CH:5][C:4]=1[C:10]([F:11])([F:12])[F:13]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 15891Phenyl chloroformateHCID 6007055-Amino-2-methoxybenzotrifluoride

생성물 1

HCID 66876756Phenyl 4-methoxy-3-(trifluoromethyl)phenylcarbamate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 4-methoxy-3-trifluoromethyl aniline (500 mg, 2.62 mmol) in 20 mL of tetrahydrofuran was added potassium carbonate (470 mg, 3.4 mmol), followed by phenyl chloroformate (532 mg, 3.4 mmol). This solution was stirred overnight at room temperature, then concentrated and purified by silica gel chromatography using a gradient of ethyl acetate/hexanes 0-20% to afford phenyl 4-methoxy-3-(trifluoromethyl)phenylcarbamate as a white solid. 1H NMR (300 MHz, CDCl3) 7.75-7.65 (m, 2H), 7.60-7.40 (m, 2H), 7.27-7.19 (m, 3H), 7.00-6.93 (m, 2H), 3.89 (s, 3H).

후처리

  1. concentrationconcentrated
  2. custompurified by silica gel chromatography

출처 및 근거

ORD 기록
ord-0f27655085ac4e9e87a7c3fbf854d704
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09320739B2

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