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

(S)-mandelic acid → (S)-1-(6-Bromo-3-methyl-5-oxo-5H-thiazolo[3,2-a]pyrimidin-7-yl)ethanaminium (S)-2-hydroxy-2-phenylacetate

HRID 58249
ノート
印刷プレビュー

反応式

HRID 58249 の反応式
[NH2:1][CH:2]([C:4]1[N:5]=[C:6]2[S:14][CH:13]=[C:12]([CH3:15])[N:7]2[C:8](=[O:11])[C:9]=1[Br:10])[CH3:3].[C:16]([OH:26])(=[O:25])[C@H:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[OH:18]>C(O)(C)C>[OH:18][C@@H:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:16]([O-:26])=[O:25].[Br:10][C:9]1[C:8](=[O:11])[N:7]2[C:12]([CH3:15])=[CH:13][S:14][C:6]2=[N:5][C:4]=1[C@@H:2]([NH3+:1])[CH3:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 439616(S)-mandelic acidHCID 581113977-(1-Aminoethyl)-6-bromo-3-methyl-5H-thiazolo[3,2-a]pyrimidin-5-one

生成物 1

HCID 86717602(S)-1-(6-Bromo-3-methyl-5-oxo-5H-thiazolo[3,2-a]pyrimidin-7-yl)ethanaminium (S)-2-hydroxy-2-phenylacetate収率 85%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

反応条件

温度
72 °C

実験手順

7-(1-Aminoethyl)-6-bromo-3-methyl-5H-thiazolo[3,2-a]pyrimidin-5-one (18.8 g, 65.2 mmol) was dissolved in isopropanol (375 mL) at reflux and then (S)-(+)-mandelic acid (4.84 g, 31.8 mmol) in isopropanol (375 mL) was added dropwise to the amine solution over 35 min. The reaction mixture was allowed to cool to about 72° C. and solid precipitation was observed. The slurry was cooled to room temperature and stirred for 1 hour. The solid product was collected by filtration. The wet cake was washed with isopropanol (100 mL) and dried on the filter under suction for 1 h to give the product (S)-1-(6-bromo-3-methyl-5-oxo-5H-thiazolo[3,2-a]pyrimidin-7-yl)ethanaminium (S)-2-hydroxy-2-phenylacetate (11.9 g) as a white solid. Chiral HPLC analysis was performed on a Lux Cellulose-2, 4.6×250 mm, 5 micron column using 60% ethanol/40% hexanes as the mobile phase at a flow rate of 1 mL/min. The major enantiomer eluted at retention time 11.21 min (99.0 area %). The minor enantiomer eluted at retention time 14.31 min (0.96 area %). The e.e. of the desired product was 98.08%.

後処理

  1. temperatureat reflux
  2. customsolid precipitation
  3. temperatureThe slurry was cooled to room temperature
  4. filtrationThe solid product was collected by filtration
  5. washThe wet cake was washed with isopropanol (100 mL)
  6. customdried on the
  7. filtrationfilter under suction for 1 h

出典と根拠

ORDレコード
ord-dbecb13b1b064a6c89803330cb0b588e
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09434746B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート