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 → N-benzoyl-L-alanyl-L-phenylalanine methyl ester

HRID 434133
ノート
印刷プレビュー

反応式

HRID 434133 の反応式
Cl.[CH3:2][O:3][C:4](=[O:14])[C@H:5]([CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[NH2:6].CN1CCOCC1.[C:22]([N:30]1[C@@H:34]([CH3:35])[C:33](=O)[O:32]C1=O)(=[O:29])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.C(N[C@H](C(O)=O)C)(=O)C1C=CC=CC=1.Cl>O1CCCC1>[CH3:2][O:3][C:4](=[O:14])[C@H:5]([CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[NH:6][C:33](=[O:32])[C@H:34]([CH3:35])[NH:30][C:22](=[O:29])[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][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

7

反応物 5

HCID 313Hydrochloric AcidHCID 79724-MethylmorpholineHCID 75736Methyl L-phenylalaninate hydrochlorideHCID 709778N-benzoyl-L-alanineHCID 9855930(S)-3-benzoyl-4-methyl-2,5-oxazolidinedione

生成物 1

HCID 59119734N-benzoyl-L-alanyl-L-phenylalanine methyl ester収率 65%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

L-Phenylalanine methyl ester hydrochloride (518 mg, 2.4 mmol) was suspended in tetrahydrofuran (12 mL), and at 0° C., N-methylmorpholine (242 mg, 2.4 mmol) was added, followed by stirring for 20 minutes. (S)-3-Benzoyl-4-methyl-2,5-oxazolidinedione (N-benzoyl-L-alanine-NCA (438 mg, 2 mmol) was added as crystals at 0° C. After the resulting mixture was stirred for 15 minutes, the mixture was allowed to rise in temperature to room temperature, at which the mixture was stirred for 15 minutes. The reaction mixture was poured into 1 N hydrochloric acid (25 mL), followed by extraction with ethyl acetate (25 mL). The organic layer was washed successively with a saturated aqueous solution of sodium hydrogencarbonate (25 mL) and a saturated aqueous solution of sodium chloride (25 mL), and was then dried over anhydrous magnesium sulfate. The organic layer was concentrated under reduced pressure. The resulting white solid was washed with hexane-ethyl acetate to afford the title compound (462 mg, 65%) as white crystals.

後処理

  1. stirringAfter the resulting mixture was stirred for 15 minutes
  2. customto rise in temperature to room temperature, at which
  3. stirringwas stirred for 15 minutes
  4. extractionfollowed by extraction with ethyl acetate (25 mL)
  5. washThe organic layer was washed successively with a saturated aqueous solution of sodium hydrogencarbonate (25 mL)
  6. dry with materiala saturated aqueous solution of sodium chloride (25 mL), and was then dried over anhydrous magnesium sulfate
  7. concentrationThe organic layer was concentrated under reduced pressure
  8. washThe resulting white solid was washed with hexane-ethyl acetate

出典と根拠

ORDレコード
ord-2d928e96782b4168bd8fe66f854af487
出典データセット
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06670447B2

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