Potassium Hydroxide → HCID 57326486, 화합물

HRID 445254노트

반응식

HRID 445254 반응식
[CH2:1]([NH:9][C:10](=O)[C:11]1[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][CH:12]=1)[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[OH-].[K+]>C(OCC)C>[F:18][C:17]([F:20])([F:19])[C:14]1[CH:15]=[CH:16][C:11]([C:10]2[C:8]3[C:3](=[CH:4][CH:5]=[CH:6][CH:7]=3)[CH2:2][CH2:1][N:9]=2)=[CH:12][CH:13]=1

참가 물질

5

반응물 3

HCID 14797Potassium Hydroxide2회HCID 14812Phosphorus oxide (P4O10)HCID 706676HCID 706676, 화합물

생성물 1

HCID 57326486HCID 57326486, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
165 °C

실험 절차

To a 100-mL round-bottomed flask was added N-phenethyl-4-(trifluoromethyl)benzamide (5.0 g, 17 mmol), phosphoric pentoxide (0.526 mL, 8.52 mmol), and polyphosphoric acid (60.0 g). The reaction mixture was heated to 165° C. for 2 h. Then, the hot solution was carefully poured into ice/water and a solution of KOH (20%, 40 mL) was added to break up the oil. The mixture was stirred at RT for 5 min and an additional amount of KOH solution was added until pH 7. Ethyl ether (250 mL) was added and the mixture was stirred at RT for 15 min. The organic layer was collected and the aqueous layer was extracted with EtOAc (2×200 mL). The combined organic extracts were dried over MgSO4 and concentrated in vacuo to give the title compound as orange oil, which was used in the next step without further purification. MS (ESI, positive ion) m/z: 276 (M+H).

후처리

  1. stirringthe mixture was stirred at RT for 15 min
  2. customThe organic layer was collected
  3. extractionthe aqueous layer was extracted with EtOAc (2×200 mL)
  4. dry with materialThe combined organic extracts were dried over MgSO4
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-0ebd8bb6af99490686f9815d1b1e2900
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08476297B2

반응 노트

불러오는 중…