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

Water → HCID 12764079、化合物

HRID 2083837
ノート
印刷プレビュー

反応式

HRID 2083837 の反応式
FC(F)(F)C(O)=O.[CH2:8]([O:15][CH2:16][C@@H:17]([C:19]([OH:21])=[O:20])[NH2:18])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.O.[O-2].[Mg+2].[CH3:25][O:26][C:27]1[CH:39]=[CH:38][C:30]([CH2:31][O:32][C:33](N=[N+]=[N-])=[O:34])=[CH:29][CH:28]=1>O1CCOCC1>[CH3:25][O:26][C:27]1[CH:39]=[CH:38][C:30]([CH2:31][O:32][C:33]([NH:18][C@H:17]([C:19]([OH:21])=[O:20])[CH2:16][O:15][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:34])=[CH:29][CH:28]=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 962WaterHCID 1175214-Methoxybenzyl azidoformateHCID 6850729Magnesium monoxideHCID 131711089HCID 131711089、化合物

生成物 1

HCID 12764079HCID 12764079、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

O-Benzyl-L-serine trifluoroacetic acid salt, 3.09 g. in 20 ml. of water containing 0.8 g. of magnesium oxide is treated with 2.28 g. of p-methoxybenzyloxycarbonyl azide in 20 ml. of dioxane. The mixture is stirred at room temperature for four days. It is then filtered and the filtrate diluted with ethyl acetate and the solution washed with cold 0.2 N hydrochloric acid and with saturated sodium chloride solution. The ethyl acetate solution is dried and evaporated to an oil. The crude product is triturated with isopropyl ether and stored in the cold to yield crystalline material. Separation by filtration gives 1.75 g., mp. 70°-72° C. This product is recrystallized from aqueous ethanol to give 1.54 g. and is again recrystallized from ethyl acetate-hexane to yield 1.25 g. of the above named product, mp. 72°-73° C.

後処理

  1. filtrationIt is then filtered
  2. additionthe filtrate diluted with ethyl acetate
  3. washthe solution washed with cold 0.2 N hydrochloric acid and with saturated sodium chloride solution
  4. dry with materialThe ethyl acetate solution is dried
  5. customevaporated to an oil
  6. customThe crude product is triturated with isopropyl ether
  7. customto yield crystalline material
  8. customSeparation
  9. filtrationby filtration
  10. customgives 1.75 g
  11. customThis product is recrystallized from aqueous ethanol
  12. customto give 1.54 g
  13. customand is again recrystallized from ethyl acetate-hexane
  14. customto yield 1.25 g

出典と根拠

ORDレコード
ord-c840487de34b484dbe9238c038f036e7
出典データセット
uspto-grants-1978_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04086219

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