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

Acetone → HCID 67582894、化合物

HRID 1416469
ノート
印刷プレビュー

反応式

HRID 1416469 の反応式
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][N:14]([C:17]2[N:26]=[C:25]([O:27][C@H]3C[C@@H](O)C=C3)[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[N:18]=2)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[N+]1([O-])CC[O:38]CC1.C[C:43]([CH3:45])=[O:44].[C:46]([OH:50])([CH3:49])([CH3:48])C>O.[Os](=O)(=O)(=O)=O>[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][N:14]([C:17]2[N:26]=[C:25]([O:27][C@H:45]3[CH2:49][C@@H:46]([OH:50])[C@H:48]([OH:38])[C@@H:43]3[OH:44])[C:24]3[C:19](=[CH:20][CH:21]=[CH:22][CH:23]=3)[N:18]=2)[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=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 180AcetoneHCID 6386tert-ButanolHCID 82029Methyl morpholine oxideHCID 67582038HCID 67582038、化合物

生成物 1

HCID 67582894HCID 67582894、化合物

試薬・触媒・溶媒 2

HCID 30318Osmium Tetroxide触媒
HCID 962
Water
溶媒

実験手順

A mixture of 2-[4-(benzyloxycarbonyl)piperazin-1-yl]-4-[(1S,4R)-(4-hydroxycyclopent-2-en-1-yl)oxy]quinazoline (1.30 g), a solution of osmium tetroxide in t-butanol (osmium tetroxide 252 mg/t-butanol 18.1 g) (532 mg) and 4-methylmorpholine N-oxide (375 mg) in water (3 ml)--acetone (25 ml) is stirred at room temperature for 17 hours. Acetone is distilled off from the reaction mixture under reduced pressure, and to the resultant is added ethyl acetate, and the mixture is washed with 10% aqueous sodium sulfite solution and water. The ethyl acetate solution is dried over anhydrous magnesium sulfate and evaporated to dryness under reduced pressure, and the residue is purified by medium pressure liquid column chromatography (eluent, chloroform:methanol=50:1, 10:1, v/v) to give 2-[4-(benzyloxycarbonyl) piperazin-1-yl]-4-[(1S,2S,3S,4R)-(2,3,4-trihydroxycyclopentan-1-yl)oxy]quinazoline (1.05 mg) as foam.

後処理

  1. distillationAcetone is distilled off from the reaction mixture under reduced pressure
  2. additionto the resultant is added ethyl acetate
  3. washthe mixture is washed with 10% aqueous sodium sulfite solution and water
  4. dry with materialThe ethyl acetate solution is dried over anhydrous magnesium sulfate
  5. customevaporated to dryness under reduced pressure
  6. customthe residue is purified by medium pressure liquid column chromatography (eluent, chloroform

出典と根拠

ORDレコード
ord-406e7175fe7640168833f420db5495f4
出典データセット
uspto-grants-1999_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05912247

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