Hydrochloric Acid → Ethyl (2s)-2-[2'-(2-bromophenyl)thio-3'-(4-methoxyphenyl)propanoyl]amino-4-methylpentanoate

HRID 50639

反応式

HRID 50639 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][CH:9]([CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=1)[C:10]([OH:12])=O.[CH2:22]([O:24][C:25](=[O:32])[C@H:26]([CH2:28][CH:29]([CH3:31])[CH3:30])[NH2:27])[CH3:23].Cl.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl>CN(C=O)C>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][CH:9]([CH2:13][C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=1)[C:10]([NH:27][C@@H:26]([CH2:28][CH:29]([CH3:30])[CH3:31])[C:25]([O:24][CH2:22][CH3:23])=[O:32])=[O:12]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 757711-HydroxybenzotriazoleHCID 75971L-Leucine ethyl esterHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 227366192-(2-Bromophenyl)thio-3-(4-methoxyphenyl)propanoic acid

生成物 1

HCID 91156048Ethyl (2s)-2-[2'-(2-bromophenyl)thio-3'-(4-methoxyphenyl)propanoyl]amino-4-methylpentanoate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2-(2-bromophenyl)thio-3-(4-methoxyphenyl)propanoic acid (1.102 g) and L-leucine ethyl ester.HCl (704 mg) in DMF (10 mL), HOBt (551 mg) and EDC.HCl (690 mg) were added. The reaction mixture was stirred at r.t. overnight. The solvent was removed under reduced pressure. The residue was dissolved in EtOAc and washed with 1N HCl, 5% Na2CO3 aq. and brine. The organic layer was dried over Na2SO4 and concentrated to give the pure product as a pale yellow oil (1.561 g, quant.).

後処理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionThe residue was dissolved in EtOAc
  3. washwashed with 1N HCl, 5% Na2CO3 aq. and brine
  4. dry with materialThe organic layer was dried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-b6ea4dc3999243a4923133973afb1594
出典データセット
uspto-grants-2004_03
特許番号
US06713477B1

関連ノート

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