ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Benzoyl chloride → (S)-9-benzoyl-2-morpholin-4-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one

HRID 80610
ノート
印刷プレビュー

反応式

HRID 80610 の反応式
[H-].[Na+].[C:3](Cl)(=[O:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[N:12]1([C:18]2[N:19]=[C:20]3[NH:28][C@H:27]([C:29]([F:32])([F:31])[F:30])[CH2:26][CH2:25][N:21]3[C:22](=[O:24])[CH:23]=2)[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1.C(=O)(O)[O-].[Na+]>O1CCCC1.C(OCC)(=O)C>[C:3]([N:28]1[C:20]2=[N:19][C:18]([N:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)=[CH:23][C:22](=[O:24])[N:21]2[CH2:25][CH2:26][C@H:27]1[C:29]([F:30])([F:31])[F:32])(=[O:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7412Benzoyl chlorideHCID 24758Sodium hydrideHCID 516892Sodium BicarbonateHCID 136238743(S)-8-(Morpholin-4-yl)-2-(trifluoromethyl)-1,2,3,4-tetrahydropyrimido[1,2-a]pyrimidin-6-one

生成物 1

HCID 49854090(S)-9-benzoyl-2-morpholin-4-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one

試薬・触媒・溶媒 2

HCID 8028
Tetrahydrofuran
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

35.7 mg of sodium hydride and then, after 10 minutes of stirring, 0.135 ml de of benzoyl chloride are added, under an argon atmosphere, to a solution of 300 mg of (S)-2-morpholin-4-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one (Example 1e) in 3 ml of tetrahydrofuran. After stirring for six hours at ambient temperature, a saturated solution of sodium bicarbonate and ethyl acetate are added to the reaction mixture. The organic phase is separated and then successively washed with a saturated solution of sodium chloride, dried over magnesium sulphate, filtered and concentrated under reduced pressure. The residue obtained is purified by silica chromatography (eluent: CH2Cl2) so as to give 74 mg of (S)-9-benzoyl-2-morpholin-4-yl-8-trifluoromethyl-6,7,8,9-tetrahydropyrimido[1,2-a]pyrimidin-4-one, in the form of a white solid, the characteristics of which are the following:

後処理

  1. customThe organic phase is separated
  2. washsuccessively washed with a saturated solution of sodium chloride
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue obtained
  7. customis purified by silica chromatography (eluent: CH2Cl2) so as

出典と根拠

ORDレコード
ord-66222c9585074824a8d726bdf81f9c07
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846670B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート