Water → 1,1-Dimethylethyl 4-[(2-nitro-3-fluoro-5-methoxyphenyl)amino]-piperidinecarboxylate

HRID 447764ノート

反応式

HRID 447764 の反応式
[N+:1]([C:4]1[C:9](F)=[CH:8][C:7]([O:11][CH3:12])=[CH:6][C:5]=1[F:13])([O-:3])=[O:2].[NH2:14][CH:15]1[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH2:16]1.O.C(OCC)(=O)C>CN(C)C=O.C(N(C(C)C)CC)(C)C>[N+:1]([C:4]1[C:5]([F:13])=[CH:6][C:7]([O:11][CH3:12])=[CH:8][C:9]=1[NH:14][CH:15]1[CH2:16][CH2:17][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:19][CH2:20]1)([O-:3])=[O:2]

参加物

7

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 12682914-Amino-1-Boc-piperidineHCID 100127101,3-Difluoro-5-methoxy-2-nitrobenzene

生成物 1

HCID 596832591,1-Dimethylethyl 4-[(2-nitro-3-fluoro-5-methoxyphenyl)amino]-piperidinecarboxylate

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 81531Diisopropylethylamine溶媒

実験手順

4-Nitro-3,5-difluoroanisole (D11) (370 mg, 2 mmol) was dissolved in dry dimethylformamide (3 ml) and diisopropylethylamine (0.4 ml), and 1,1-dimethylethyl 4-amino-1-piperidinecarboxylate (400 mg, 2 mmol) were added at room temperature. The mixture was stirred at room temperature for 18 h, then cooled to room temperature and water and ethyl acetate added. The organic layer was dried over MgSO4, filtered and evaporated, and the residue crystallised from diethyl ether to afford the title compound, 380 mg. M−−H=368.

後処理

  1. temperaturecooled to room temperature
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. customevaporated
  5. customthe residue crystallised from diethyl ether

出典と根拠

ORDレコード
ord-2d7926662dc641918f85cc3e449e5200
出典データセット
uspto-grants-2013_07
特許番号
US08481566B2

反応ノート

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