N-[3,5-bis(trifluoromethyl)benzyl]-N-[3-(t-butoxycarbonylamino)propyl]-4,6-dichloro-2-(methylthio)pyrimidine-5-carboxylic acid amide → N-[3,5-bis(trifluoromethyl)benzyl]-N-(3-aminopropyl)-4,6-dichloro-2-(methylthio)pyrimidine-5-carboxylic acid amide hydrochloride

HRID 1829639ノート

反応式

HRID 1829639 の反応式
[F:1][C:2]([F:39])([F:38])[C:3]1[CH:4]=[C:5]([CH:31]=[C:32]([C:34]([F:37])([F:36])[F:35])[CH:33]=1)[CH2:6][N:7]([CH2:20][CH2:21][CH2:22][NH:23]C(OC(C)(C)C)=O)[C:8]([C:10]1[C:11]([Cl:19])=[N:12][C:13]([S:17][CH3:18])=[N:14][C:15]=1[Cl:16])=[O:9]>C(OCC)(=O)C.Cl>[ClH:16].[F:38][C:2]([F:1])([F:39])[C:3]1[CH:4]=[C:5]([CH:31]=[C:32]([C:34]([F:37])([F:36])[F:35])[CH:33]=1)[CH2:6][N:7]([CH2:20][CH2:21][CH2:22][NH2:23])[C:8]([C:10]1[C:11]([Cl:19])=[N:12][C:13]([S:17][CH3:18])=[N:14][C:15]=1[Cl:16])=[O:9]

参加物

3

反応物 1

HCID 21030672N-[3,5-bis(trifluoromethyl)benzyl]-N-[3-(t-butoxycarbonylamino)propyl]-4,6-dichloro-2-(methylthio)pyrimidine-5-carboxylic acid amide

生成物 1

HCID 86599717N-[3,5-bis(trifluoromethyl)benzyl]-N-(3-aminopropyl)-4,6-dichloro-2-(methylthio)pyrimidine-5-carboxylic acid amide hydrochloride収率 199%

試薬・触媒・溶媒 1

HCID 21866389Hydrogen chloride-ethyl acetate溶媒

実験手順

3 mol/L hydrogen chloride-ethyl acetate (20 mL) was added to N-[3,5-bis(trifluoromethyl)benzyl]-N-[3-(t-butoxycarbonylamino)propyl]-4,6-dichloro-2-(methylthio)pyrimidine-5-carboxylic acid amide (Compound of Reference Example 4; 8.23 g) while the solution was chilled on an ice bath. The reaction mixture was stirred for 1 hour and then another 1 hour at room temperature. Subsequently, the solvent was removed to obtain N-[3,5-bis(trifluoromethyl)benzyl]-N-(3-aminopropyl)-4,6-dichloro-2-(methylthio)pyrimidine-5-carboxylic acid amide hydrochloride (7.35 g, 100%).

後処理

  1. temperaturewas chilled on an ice bath
  2. customanother 1 hour
  3. customat room temperature
  4. customSubsequently, the solvent was removed

出典と根拠

ORDレコード
ord-f4433cd8aeee4830b8e056d819810579
出典データセット
uspto-grants-2006_06
特許番号
US07064119B2

反応ノート

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