tert-Butyl carbazate → N'-(4-methoxybutyryl)hydrazine carboxylic acid tert-butyl ester

HRID 6924

反応式

HRID 6924 の反応式
[C:1]([O:5][C:6](=[O:9])[NH:7][NH2:8])([CH3:4])([CH3:3])[CH3:2].[CH3:10][O:11][CH2:12][CH2:13][CH2:14][C:15](O)=[O:16].Cl.C(N=C=NCCCN(C)C)C>N1C=CC=CC=1>[C:1]([O:5][C:6]([NH:7][NH:8][C:15](=[O:16])[CH2:14][CH2:13][CH2:12][O:11][CH3:10])=[O:9])([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 70091tert-Butyl carbazateHCID 922644-Methoxybutyric acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 86594808N'-(4-methoxybutyryl)hydrazine carboxylic acid tert-butyl ester

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Carbazic acid tert-butyl ester (9.21 g) was dissolved in pyridine (120 ml), followed by addition of 4-methoxybutyric acid (9.06 g) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride salt (20.0 g), and stirred at ambient temperature for 64 hours. After the reaction solution was concentrated under reduced pressure, ethyl acetate was added to the residue, which was then washed with aqueous 1 mol/liter hydrochloric acid solution, saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride, and dried over anhydrous sodium sulfate. After the solvent was evaporated under reduced pressure, N′-(4-methoxybutyryl)hydrazine carboxylic acid tert-butyl ester was obtained in yellow oil (9.30 g, 57%). The physico-chemical values are as follows.

後処理

  1. concentrationAfter the reaction solution was concentrated under reduced pressure, ethyl acetate
  2. additionwas added to the residue, which
  3. washwas then washed with aqueous 1 mol/liter hydrochloric acid solution, saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. customAfter the solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-23a7463ec365497a8da5e62103007ce0
出典データセット
uspto-grants-2006_08
特許番号
US07084164B2

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