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

4-Methylmorpholine → Methyl 3-(4-chlorophenyl)-2-formamidopropanoate

HRID 902835
ノート
印刷プレビュー

反応式

HRID 902835 の反応式
[ClH:1].[CH3:2][O:3][C:4](=[O:15])[C@H:5]([CH3:14])[NH:6][C:7]1C=CC(Cl)=CC=1.Cl.CN(C)CCCN=C=NCC.[OH2:28].ON1[C:34]2[CH:35]=[CH:36][CH:37]=[CH:38][C:33]=2N=N1.CN1CCOCC1>C(Cl)Cl.C(O)=O>[Cl:1][C:33]1[CH:38]=[CH:37][C:36]([CH2:14][CH:5]([NH:6][CH:7]=[O:28])[C:4]([O:3][CH3:2])=[O:15])=[CH:35][CH:34]=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 79724-MethylmorpholineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 67056399(+/-)-(4-Chlorophenyl)alanine methyl ester hydrochloride

生成物 1

HCID 14318072Methyl 3-(4-chlorophenyl)-2-formamidopropanoate収率 62.6%

試薬・触媒・溶媒 2

HCID 284Formic Acid溶媒2 回
HCID 6344Dichloromethane溶媒2 回

実験手順

(±)-(4-Chlorophenyl)alanine methyl ester hydrochloride (2.00 g) was suspended in methylene chloride (20 ml), and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.60 g), 1-hydroxybenzotriazole monohydrate (1.23 g), N-methylmorpholine (1.90 ml) and formic acid (0.30 ml) were added to stir the mixture for 15 minutes. After a process in which formic acid (0.30 ml) was additionally added to stir the mixture for 15 minutes was repeated 3 times, the reaction mixture was diluted with methylene chloride. After an ogranic layer was washed with water and then dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The residue was purified by column chromatography on silica gel (methylene chloride:methanol=40:1) to obtain the title compound (1.21 g).

後処理

  1. stirringto stir the mixture for 15 minutes
  2. washAfter an ogranic layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (methylene chloride:methanol=40:1)

出典と根拠

ORDレコード
ord-aa83c700fa0e42fcab14e01fcf792750
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07365205B2

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