Trifluoroacetic acid → HCID 67915874、化合物

HRID 1029934ノート

反応式

HRID 1029934 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 67915874HCID 67915874、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1469b5e7a23d4e4081561e217425932c
出典データセット
uspto-grants-1992_04
特許番号
US05102667

反応ノート

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