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

Hydrochloric Acid → (2S)-7-hydroxy-2-methyl-2-(trifluoromethyl)-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one

HRID 633710
ノート
印刷プレビュー

反応式

HRID 633710 の反応式
Br.[CH3:2][C@@:3]1([C:9]([F:12])([F:11])[F:10])[CH2:7][NH:6][C:5]([NH2:8])=[N:4]1.C[O-].[Na+].[C:16](OCC)(=[O:23])[CH2:17][C:18](OCC)=[O:19].Cl>CO>[OH:23][C:16]1[N:8]=[C:5]2[NH:4][C@:3]([CH3:2])([C:9]([F:12])([F:10])[F:11])[CH2:7][N:6]2[C:18](=[O:19])[CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7761Diethyl MalonateHCID 10942334Sodium MethoxideHCID 178419517HCID 178419517、化合物

生成物 1

HCID 136069601(2S)-7-hydroxy-2-methyl-2-(trifluoromethyl)-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one収率 107.5%

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

36.90 g (148.76 mmol) of (S)-4-methyl-4-trifluoromethyl-4,5-dihydro-1H-imidazol-2-ylamine hydrobromide and 24.10 g (446 mmol) of sodium methoxide are added to a mixture of 29.50 g (216.43 mmol) of diethyl malonate in 200 mL of methanol. The resulting mixture is refluxed for 18 hours. After cooling, the mixture obtained is concentrated to dryness under vacuum. 65 mL of cold water are added to the residue obtained, to obtain a thick suspension, to which is added 25% hydrochloric acid to pH 5. The resulting suspension is stirred in an ice bath for 3 hours and then filtered. The insoluble matter obtained is rinsed with water and then dried to give 37.60 g of (S)-7-hydroxy-2-methyl-2-trifluoromethyl-2,3-dihydro-1H-imidazo[1,2-a]pyrimidin-5-one in the form of a white solid, the characteristics of which are as follows:

後処理

  1. temperatureThe resulting mixture is refluxed for 18 hours
  2. temperatureAfter cooling
  3. customthe mixture obtained
  4. concentrationis concentrated to dryness under vacuum
  5. addition65 mL of cold water are added to the residue
  6. customobtained
  7. customto obtain a thick suspension
  8. filtrationfiltered
  9. customThe insoluble matter obtained
  10. washis rinsed with water
  11. customdried

出典と根拠

ORDレコード
ord-43503273fe1b44dd9d333b8bf87d22e6
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09321790B2

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