Trifluoroacetic acid → HCID 67915874, 화합물

HRID 1029934노트

반응식

HRID 1029934 반응식
FC(F)(F)C(O)=O.[F:8][C:9]1[CH:10]=[C:11]([C:15]2([C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([F:28])[CH:23]=3)[CH2:20][CH2:19][C:18](=[O:21])[CH:17]=[CH:16]2)[CH:12]=[CH:13][CH:14]=1.C(O[CH2:34][N:35]([CH2:41][C:42]1[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1)[CH2:36][Si](C)(C)C)CCC.C(=O)([O-])[O-].[K+].[K+]>ClCCl>[CH2:41]([N:35]1[CH2:36][CH:17]2[CH:16]([C:15]([C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([F:28])[CH:23]=3)([C:11]3[CH:12]=[CH:13][CH:14]=[C:9]([F:8])[CH:10]=3)[CH2:20][CH2:19][C:18]2=[O:21])[CH2:34]1)[C:42]1[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1

참가 물질

6

반응물 4

HCID 6422Trifluoroacetic acidHCID 11430Potassium CarbonateHCID 11097910N-Benzyl-1-butoxy-N-[(trimethylsilyl)methyl]methanamineHCID 543073284,4-Bis(3-fluorophenyl)cyclohexenone

생성물 1

HCID 67915874HCID 67915874, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic acid (3 cc) is added to a solution of 4,4-bis-(3-fluorophenyl)cyclohexenone (90.3 g) and N-butoxymethyl-N-trimethylsilylmethylbenzylamine (123 cc) in dry dichloromethane (1,000 cc). The reaction mixture is brought to reflux and then stirred for 2 hours allowing the temperature to return to 25° C. and is then stirred for a further 15 minutes after addition of potassium carbonate (60 g). After filtering and concentrating the filtrate to dryness under reduced pressure (2.7 kPa), the crystallized residue is scraped with isopropyl ether, drained, washed and recrystallized from cyclohexane (300 cc). The crystals are drained, washed with cyclohexane (2×15 cc) and dried to give (3aRS,7aRS)-2-benzyl-7,7-bis-(3-fluorophenyl)-4-perhydroisoindolone (92 g) in the form of white crystals. m.p.=124° C.

후처리

  1. temperatureto reflux
  2. customto return to 25° C.
  3. stirringis then stirred for a further 15 minutes
  4. filtrationAfter filtering
  5. concentrationconcentrating the filtrate to dryness under reduced pressure (2.7 kPa)
  6. washwashed
  7. customrecrystallized from cyclohexane (300 cc)
  8. washwashed with cyclohexane (2×15 cc)
  9. customdried

출처 및 근거

ORD 기록
ord-1469b5e7a23d4e4081561e217425932c
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05102667

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