Methyl chloroformate → HCID 21993429, 화합물

HRID 1977581노트

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HRID 1977581 반응식
[CH:1]1([CH2:5][CH:6]([C:8]([OH:10])=[O:9])[NH2:7])[CH2:4][CH2:3][CH2:2]1.Cl[C:12]([O:14][CH3:15])=[O:13]>[OH-].[Na+].O>[CH3:15][O:14][C:12]([NH:7][CH:6]([C:8]([OH:10])=[O:9])[CH2:5][CH:1]1[CH2:4][CH2:3][CH2:2]1)=[O:13]

참가 물질

5

반응물 2

HCID 6586Methyl chloroformateHCID 219880662-Amino-3-cyclobutylpropanoic acid

생성물 1

HCID 21993429HCID 21993429, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 14798Sodium Hydroxide용매2회

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온도
0 °C

실험 절차

4.3 g (30 mmol) of 3-cyclobutyl-DL-alanine [A. Burger et al., J. Med. Chem. 6, 221 (1963)] is dissolved in 15 ml of 2M NaOH solution, cooled to 0° C. and simultaneously 16.5 ml of 2M NaOH solution and 2.55 ml (33 mmol) of methyl chloroformate are added with vigorous stirring. Stirring is continued at this temperature for 30 minutes and at room temperature for 2 hours. The reaction mixture is diluted with 40 ml of water, extracted with 10 ml of diethyl ether, then acidified to pH3 with 3M HCl. The product is extracted with ethyl acetate (4×20 ml), the extracts are pooled, washed with 20 ml of water, dried over anhydrous sodium sulphate and evaporated at a pressure of 2.0-2.5 kPa. The oily residue [5.3 g (88%), Rf(7)=0.61] is used without further purification in the next step.

후처리

  1. extractionextracted with 10 ml of diethyl ether
  2. extractionThe product is extracted with ethyl acetate (4×20 ml)
  3. washwashed with 20 ml of water
  4. dry with materialdried over anhydrous sodium sulphate
  5. customevaporated at a pressure of 2.0-2.5 kPa
  6. customThe oily residue [5.3 g (88%), Rf(7)=0.61] is used without further purification in the next step

출처 및 근거

ORD 기록
ord-0db29f9e9a3a46348dc3bda1d2484ac9
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235707B1

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