Potassium Carbonate → N-acryloylasparagineamide

HRID 2261500

반응식

HRID 2261500 반응식
[C:1](Cl)(=[O:4])[CH:2]=[CH2:3].Cl.[NH2:7][C@H:8]([C:13]([NH2:15])=[O:14])[CH2:9][C:10](=[O:12])[NH2:11].C(=O)([O-])[O-].[K+].[K+].N[C@H](C(N)=O)CC(=O)N>O.C(OCC)C>[C:1]([NH:15][C:13](=[O:14])[C@H:8]([CH2:9][C:10](=[O:12])[NH2:11])[NH2:7])(=[O:4])[CH:2]=[CH2:3]

참가 물질

7

반응물 4

HCID 11430Potassium Carbonate2회HCID 13140Acryloyl chlorideHCID 447212AsparaginamideHCID 16218940(S)-2-Aminosuccinamide hydrochloride

생성물 1

HCID 86614804N-acryloylasparagineamide

시약·촉매·용매 2

HCID 962Water용매2회HCID 3283Diethyl Ether용매2회

실험 절차

A 5 ml portion of acrylic acid chloride and 200 ml of diethyl ether were put into a 500 ml capacity eggplant type flask and stirred on an ice bath. Next, 1.84 g of asparagineamide hydrochloride (mfd. by Kokusan Kagaku) was dissolved in 40 ml of deionized water, and 3 g of potassium carbonate was dissolved in 20 ml of deionized water. The asparagineamide aqueous solution was mixed with the potassium carbonate aqueous solution. The mixed liquid was added dropwise into the eggplant type flask spending 10 minutes while stirring constantly, and the mixture after completion of the dropwise addition was stirred for 24 hours. Diethyl ether layer in the thus obtained reaction liquid was discarded, and the water layer was concentrated at 25° C. under a reduced pressure. One liter of acetone was added to the thus obtained residue and stirred for 1 hour. The insoluble solids were removed by suction filtration. By recrystallizing from the acetone layer, 0.5 g of colorless crystals were obtained.

후처리

  1. additionThe mixed liquid was added dropwise into the eggplant type flask
  2. stirringwhile stirring constantly
  3. additionthe mixture after completion of the dropwise addition
  4. stirringwas stirred for 24 hours
  5. concentrationthe water layer was concentrated at 25° C. under a reduced pressure
  6. additionOne liter of acetone was added to the thus obtained residue
  7. stirringstirred for 1 hour
  8. customThe insoluble solids were removed by suction filtration
  9. customBy recrystallizing from the acetone layer

출처 및 근거

ORD 기록
ord-6ed8b20100954c9fa06fccad7e233979
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07847047B2

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