Tetrahydrofuran → 1-tert-Butyl 3-methyl 4-[5-(4-chlorobenzyl)-4-oxo-4,5-dihydro-1,3,5-triazin-2-yl]piperazine-1,3-dicarboxylate

HRID 1477612ノート

反応式

HRID 1477612 の反応式
O1CCCC1.[N:6]1([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:11][CH2:10][NH:9][CH:8]([C:12]([O:14][CH3:15])=[O:13])[CH2:7]1.C(=O)([O-])[O-].[Na+].[Na+].Cl[C:30]1[N:35]=[CH:34][N:33]([CH2:36][C:37]2[CH:42]=[CH:41][C:40]([Cl:43])=[CH:39][CH:38]=2)[C:32](=[O:44])[N:31]=1>O>[Cl:43][C:40]1[CH:41]=[CH:42][C:37]([CH2:36][N:33]2[CH:34]=[N:35][C:30]([N:9]3[CH2:10][CH2:11][N:6]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:7][CH:8]3[C:12]([O:14][CH3:15])=[O:13])=[N:31][C:32]2=[O:44])=[CH:38][CH:39]=1

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 10340Sodium CarbonateHCID 27568191-tert-Butyl 3-methyl piperazine-1,3-dicarboxylateHCID 1178396204-chloro-1-(4-chlorobenzyl)-1,3,5-triazin-2(1H)-one

生成物 1

HCID 1178398111-tert-Butyl 3-methyl 4-[5-(4-chlorobenzyl)-4-oxo-4,5-dihydro-1,3,5-triazin-2-yl]piperazine-1,3-dicarboxylate収率 43.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To tetrahydrofuran solution (2.3 mL) of 1-tert-butyl 3-methyl piperazine-1,3-dicarboxylate (43 mg, 0.17 mmol), sodium carbonate (37 mg, 0.35 mmol) and 4-chloro-1-(4-chlorobenzyl)-1,3,5-triazin-2(1H)-one (45 mg, 0.17 mmol) synthesized in Reference Synthesis Example 11 were added and the resultant solution was stirred at room temperature for 1 day. After completion of the reaction, water was added thereto and extraction with chloroform from the resultant mixture was performed three times. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure and ethyl acetate was added to the obtained residue. The obtained solid was collected by filtration and dried under reduced pressure to obtain the title compound (34 mg, yield 42%).

後処理

  1. additionwere added
  2. additionwas added
  3. extractionextraction with chloroform from the resultant mixture
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure and ethyl acetate
  7. additionwas added to the obtained residue
  8. filtrationThe obtained solid was collected by filtration
  9. customdried under reduced pressure

出典と根拠

ORDレコード
ord-6dc87ce909464561a9176036227b3e44
出典データセット
uspto-grants-2016_08
特許番号
US09403798B2

反応ノート

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