3-(Trifluoromethyl)piperidine → 2-Amino-3-nitro-6-(3-trifluoromethyl-piperidin-1-yl)benzonitrile

HRID 1258715ノート

反応式

HRID 1258715 の反応式
[NH2:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[C:6](F)[C:3]=1[C:4]#[N:5].[F:14][C:15]([F:23])([F:22])[CH:16]1[CH2:21][CH2:20][CH2:19][NH:18][CH2:17]1>C1COCC1>[NH2:1][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[C:6]([N:18]2[CH2:19][CH2:20][CH2:21][CH:16]([C:15]([F:23])([F:22])[F:14])[CH2:17]2)[C:3]=1[C:4]#[N:5]

参加物

4

反応物 2

HCID 27607763-(Trifluoromethyl)piperidineHCID 679578082-Amino-6-fluoro-3-nitrobenzonitrile

生成物 1

HCID 679579752-Amino-3-nitro-6-(3-trifluoromethyl-piperidin-1-yl)benzonitrile

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 2-amino-6-fluoro-3-nitrobenzonitrile (3.1 g, 17 mmol), 3-trifluoromethylpiperidine (2.5 g, 19 mmol), TEA (3.4 g, 34 mmol) and THF (110 mL) was stirred under Ar at rt for 3 h. The mixture was concentrated and poured into H2O and thereafter extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. Crystallization from EtOAc gave the sub-title compound.

後処理

  1. concentrationThe mixture was concentrated
  2. additionpoured into H2O
  3. extractionextracted with EtOAc
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customCrystallization from EtOAc

出典と根拠

ORDレコード
ord-b2aca5afa59748e991f079ff9947731b
出典データセット
uspto-grants-2013_06
特許番号
US08466186B2

反応ノート

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