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Hydrochloric Acid → HCID 54437783、化合物

HRID 1374985
ノート
印刷プレビュー

反応式

HRID 1374985 の反応式
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:15][O:16][C:17](=[O:34])[C@H:18]([NH:29][C:30](=[O:33])[CH2:31]Cl)[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([CH3:26])=[C:22]([O:27][CH3:28])[CH:21]=1.Cl>CN(C)C=O.ClCCl>[CH3:15][O:16][C:17](=[O:34])[C@H:18]([NH:29][C:30](=[O:33])[CH2:31][NH:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([CH3:26])=[C:22]([O:27][CH3:28])[CH:21]=1
参加物反応条件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 313Hydrochloric AcidHCID 7504BenzylamineHCID 11430Potassium CarbonateHCID 54076724HCID 54076724、化合物

生成物 1

HCID 54437783HCID 54437783、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒
HCID 6344
Dichloromethane
溶媒

反応条件

温度
35 °C

実験手順

Benzylamine (1.65 g) and potassium carbonate (1.28 g) were added successively to a solution of (2R)-2-[N-(chloroacetyl)amino]-3-(3-methoxy-4-methylphenyl)propionic acid methyl ester (1.85 g) in N,N-dimethylformamide (15 ml) at 20° C. After being stirred at 35° C. for 1.5 hours, the mixture was poured into a mixture of ice-water (20 ml) and dichloromethane (20 ml). After the mixture was adjusted to pH 9 with diluted aqueous hydrochloric acid under stirring, the organic layer was separated, washed with brine (20 ml), dried over magnesium sulfate and evaporated under reduced pressure to give an oil of (2R)-2-[N-(benzylaminoacetyl)-amino]-3-(3-methoxy-4-methylphenyl)propionic acid methyl ester. A solution of (2R)-2-[N-(benzylaminoacetyl)amino]-3-(3-methoxy-4-methylphenyl)propionic acid methyl ester obtained by above procedure and acetic acid (0.18 ml) in isopropyl alcohol (10 ml) was stirred for 12 hours under reflux.

後処理

  1. stirringunder stirring
  2. customthe organic layer was separated
  3. washwashed with brine (20 ml)
  4. dry with materialdried over magnesium sulfate
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-2780cb9309fa430c996dc542320aff99
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07166598B2

反応ノート

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