3,5-Bis(trifluoromethyl)phenyl isocyanate → Tert-butyl 4-[1-({[3,5-bis(trifluoromethyl)phenyl]amino}carbonyl)azetidin-3-yl]piperazine-1-carboxylate

HRID 1788350ノート

反応式

HRID 1788350 の反応式
[NH:1]1[CH2:4][CH:3]([N:5]2[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]2)[CH2:2]1.[N:18]([C:21]1[CH:26]=[C:25]([C:27]([F:30])([F:29])[F:28])[CH:24]=[C:23]([C:31]([F:34])([F:33])[F:32])[CH:22]=1)=[C:19]=[O:20]>O1CCCC1>[F:28][C:27]([F:29])([F:30])[C:25]1[CH:26]=[C:21]([NH:18][C:19]([N:1]2[CH2:4][CH:3]([N:5]3[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]3)[CH2:2]2)=[O:20])[CH:22]=[C:23]([C:31]([F:34])([F:32])[F:33])[CH:24]=1

参加物

4

反応物 2

HCID 27333143,5-Bis(trifluoromethyl)phenyl isocyanateHCID 21183794tert-Butyl 4-(azetidin-3-yl)piperazine-1-carboxylate

生成物 1

HCID 23140263Tert-butyl 4-[1-({[3,5-bis(trifluoromethyl)phenyl]amino}carbonyl)azetidin-3-yl]piperazine-1-carboxylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of the compound prepared in Example 2 (986 mg) in tetrahydrofuran (12 mL) was dropwise added 1-isocyanato-3,5-bis(trifluoromethyl)benzene (0.85 mL), and the mixture was stirred for 30 minutes. The reaction solution was concentrated. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1) to give the compound of the present invention (1.413 g) having the following physical data.

後処理

  1. concentrationThe reaction solution was concentrated
  2. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1)
  3. customto give the compound of the present invention (1.413 g)

出典と根拠

ORDレコード
ord-4559a6888c6b47bd998d55458b50c4ed
出典データセット
uspto-grants-2009_03
特許番号
US07511159B2

反応ノート

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