Triethylamine → N2-[4-(dimethylphosphoryl)phenyl]-N4-(hexahydrocyclopenta[c]pyrrol-2(1H)-yl)-5-(trifluoromethyl)pyrimidine-2,4-diamine

HRID 921284

反応式

HRID 921284 の反応式
Cl[C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][N:5]=[C:4]([NH:12][C:13]2[CH:18]=[CH:17][C:16]([P:19]([CH3:22])([CH3:21])=[O:20])=[CH:15][CH:14]=2)[N:3]=1.C(N(CC)CC)C.Cl.[NH2:31][N:32]1[CH2:39][CH:38]2[CH:34]([CH2:35][CH2:36][CH2:37]2)[CH2:33]1>C(O)C>[CH3:21][P:19]([C:16]1[CH:17]=[CH:18][C:13]([NH:12][C:4]2[N:3]=[C:2]([NH:31][N:32]3[CH2:39][CH:38]4[CH2:37][CH2:36][CH2:35][CH:34]4[CH2:33]3)[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][N:5]=2)=[CH:14][CH:15]=1)([CH3:22])=[O:20]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 16213802Hexahydrocyclopenta(c)pyrrol-2(1H)-amine monohydrochlorideHCID 86668788HCID 86668788、化合物

生成物 1

HCID 68165214N2-[4-(dimethylphosphoryl)phenyl]-N4-(hexahydrocyclopenta[c]pyrrol-2(1H)-yl)-5-(trifluoromethyl)pyrimidine-2,4-diamine収率 67%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 4-chloro-N-[4-(dimethylphosphoryl)phenyl]-5-(trifluoromethyl)pyrimidin-2-amine (prepared as in Example 1: 40 mg, 0.12 mmol) in 2 mL of ethanol was added 50 L of triethylamine and 3-Amino-3-azabicyclo-[3,3,0]octane hydrochloride salt (19 mg, 0.12 mmol). The mixture was microwave at 120 degrees for 20 minutes. The reaction mixture was filtered through a syringe filter and purified by prep-HPLC (Waters Sunfire C18 column with ACN/water mobile phases) to yield a white solid as product (34 mg, 67% yield.) MS/ES+: m/z=440.

後処理

  1. customat 120 degrees
  2. customfor 20 minutes
  3. filtrationThe reaction mixture was filtered through a syringe
  4. filtrationfilter
  5. custompurified by prep-HPLC (Waters Sunfire C18 column with ACN/water mobile phases)
  6. customto yield a white solid as product (34 mg, 67% yield.) MS/ES+

出典と根拠

ORDレコード
ord-cb1cc0781b284f1aa6292ba04c67b9d7
出典データセット
uspto-grants-2016_03
特許番号
US09273077B2

関連ノート

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