2-Tert-Butylphenol → 2-(2-Tert-butylphenoxy)-3-nitrothiophene

HRID 555429

반응식

HRID 555429 반응식
Cl[C:2]1[S:3][CH:4]=[CH:5][C:6]=1[N+:7]([O-:9])=[O:8].[C:10]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[OH:20])([CH3:13])([CH3:12])[CH3:11].C([O-])([O-])=O.[K+].[K+]>CN1C(=O)CCC1>[C:10]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[O:20][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[N+:7]([O-:9])=[O:8])([CH3:13])([CH3:11])[CH3:12]

참가 물질

5

반응물 3

HCID 69232-Tert-ButylphenolHCID 11430Potassium CarbonateHCID 2201862-Chloro-3-nitrothiophene

생성물 1

HCID 598573712-(2-Tert-butylphenoxy)-3-nitrothiophene

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
105 °C

실험 절차

To a solution of 2-chloro-3-nitrothiophene (1.13 g, 6.93 mmol) in NMP (10 mL) in a pressure vessel was added 2-tert-butylphenol (1.04 g, 6.93 mmol) and K2CO3 (1.0 g, 10.1 mmol). The reaction was flushed with nitrogen, sealed and then heated to 105° C. for 48 h. The reaction was cooled to rt, diluted with EtOAc (˜150 mL) and washed twice with saturated aqueous NaCl (2ט150 mL). The aqueous washes were then back extracted with EtOAc. The combined organics were dried over MgSO4, filtered and concentrated to yield the crude desired product.

후처리

  1. customThe reaction was flushed with nitrogen
  2. customsealed
  3. temperatureThe reaction was cooled to rt
  4. additiondiluted with EtOAc (˜150 mL)
  5. washwashed twice with saturated aqueous NaCl (2ט150 mL)
  6. extractionThe aqueous washes were then back extracted with EtOAc
  7. dry with materialThe combined organics were dried over MgSO4
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-eb9dfcffa5234e0e81072bfdd967b62b
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08053450B2

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