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4-(Trifluoromethyl)benzoic acid → HCID 58071748、化合物

HRID 1631905
ノート
印刷プレビュー

反応式

HRID 1631905 の反応式
C([O:5][C:6](=[O:25])[CH2:7][C:8]1[C:9]([CH2:23][CH3:24])=[N:10][N:11]([CH2:15][C:16]2[CH:21]=[CH:20][C:19]([NH2:22])=[CH:18][CH:17]=2)[C:12]=1[CH2:13][CH3:14])(C)(C)C.[F:26][C:27]([F:38])([F:37])[C:28]1[CH:36]=[CH:35][C:31]([C:32](O)=[O:33])=[CH:30][CH:29]=1.C(N(C(C)C)CC)(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C([O-])([O-])=O.[K+].[K+]>CN(C)C=O>[CH2:23]([C:9]1[C:8]([CH2:7][C:6]([OH:5])=[O:25])=[C:12]([CH2:13][CH3:14])[N:11]([CH2:15][C:16]2[CH:17]=[CH:18][C:19]([NH:22][C:32](=[O:33])[C:31]3[CH:35]=[CH:36][C:28]([C:27]([F:26])([F:37])[F:38])=[CH:29][CH:30]=3)=[CH:20][CH:21]=2)[N:10]=1)[CH3:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 99664-(Trifluoromethyl)benzoic acidHCID 11430Potassium CarbonateHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 66707286HCID 66707286、化合物2 回

生成物 1

HCID 58071748HCID 58071748、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Coupling: To a solution of [1-(4-amino-benzyl)-3,5-diethyl-1H-pyrazol-4-yl]-acetic acid tert-butyl ester (intermediate 2.1.2, 99 mg, 0.29 mmol) in dimethylformamide (1.5 mL) was added 4-(trifluoromethyl)benzoic acid (67 mg, 0.34 mmol), diisopropylethylamine (90 μL, 0.53 mmol) and TBTU (82 mg, 0.25 mmol). The reaction mixture was stirred for 18 h at room temperature. The reaction mixture was treated with aqueous K2CO3 solution (2 M, 0.15 mL) and filtered over Alox B, eluting with 10% methanol in dichloromethane. Cleavage of tert-butyl ester: The volatiles were removed under reduced pressure and the residue was treated with trifluoroacetic acid (2 mL). After 42 h, the mixture was concentrated under reduced pressure and purified via preparative reversed phase HPLC (gradient of methanol in water+0.1% NH3).

後処理

  1. filtrationfiltered over Alox B
  2. washeluting with 10% methanol in dichloromethane
  3. customCleavage of tert-butyl ester: The volatiles were removed under reduced pressure
  4. additionthe residue was treated with trifluoroacetic acid (2 mL)
  5. waitAfter 42 h
  6. concentrationthe mixture was concentrated under reduced pressure
  7. custompurified via preparative reversed phase HPLC (gradient of methanol in water+0.1% NH3)

出典と根拠

ORDレコード
ord-595de646f3cc4ef5a1c6a8044b97e662
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08791272B2

反応ノート

読み込み中…

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