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O-Methyltyramine → HCID 36760427、化合物

HRID 1876283
ノート
印刷プレビュー

反応式

HRID 1876283 の反応式
Cl.C(N=C=NCCCN(C)C)C.[C:13]([O:17][C:18]([N:20]1[CH2:24][CH2:23][CH2:22][C@H:21]1[C:25]([OH:27])=O)=[O:19])([CH3:16])([CH3:15])[CH3:14].[CH3:28][O:29][C:30]1[CH:38]=[CH:37][C:33]([CH2:34][CH2:35][NH2:36])=[CH:32][CH:31]=1.C(N(C(C)C)CC)(C)C.ON1C2C=CC=CC=2N=N1>C(Cl)Cl>[C:13]([O:17][C:18]([N:20]1[CH2:24][CH2:23][CH2:22][C@H:21]1[C:25](=[O:27])[NH:36][CH2:35][CH2:34][C:33]1[CH:37]=[CH:38][C:30]([O:29][CH3:28])=[CH:31][CH:32]=1)=[O:19])([CH3:14])([CH3:15])[CH3:16]
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 4657O-MethyltyramineHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 850831,2-Pyrrolidinedicarboxylic acid, 1-(1,1-dimethylethyl) ester, (2S)-HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 36760427HCID 36760427、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

18.9 g of N-(Ethyl-N′-(3-dimethylaminopropyl)carbodiimide hydrochloride are added to a cooled solution of 20.04 g of (S)-Pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester, 14.9 g of 4-methoxyphenethylamine, 16.9 ml of diisopropylethylamine and 13.2 g of 1-hydroxy-benzotriazole in 250 ml of CH2Cl2. The reaction mixture obtained is stirred at rt for 16 hours, the reaction is quenched with aq. 2N HCl solution and the aq. phase obtained is extracted with CH2Cl2. The combined organic phases obtained are washed with aq. 2N HCl solution, brine and aq. saturated NaHCO3 solution, dried and solvent is evaporated. The residue obtained is purified by recrystallisation with EtOAc/hexane (1/3) to afford the title compound.

後処理

  1. customThe reaction mixture obtained
  2. customthe reaction is quenched with aq. 2N HCl solution
  3. customthe aq. phase obtained
  4. extractionis extracted with CH2Cl2
  5. customThe combined organic phases obtained
  6. washare washed with aq. 2N HCl solution, brine and aq. saturated NaHCO3 solution
  7. customdried
  8. customsolvent is evaporated
  9. customThe residue obtained
  10. customis purified by recrystallisation with EtOAc/hexane (1/3)

出典と根拠

ORDレコード
ord-92ea93b2d50247039d1a5f3c6eb8b9f5
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08309596B2

反応ノート

読み込み中…

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