Sodium Acetate → HCID 178513824, 화합물

HRID 514679

반응식

HRID 514679 반응식
O.O.Cl.[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11].C([O-])(=O)C.[Na+]>Cl>[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11]

참가 물질

4

반응물 2

HCID 517045Sodium AcetateHCID 178479550HCID 178479550, 화합물

생성물 1

HCID 178513824HCID 178513824, 화합물수율 95.8%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
45 °C

실험 절차

Under the nitrogen atmosphere, 10.0 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate prepared according to the method of Reference Example 2 was added to 120 mL of 0.45 mol/L hydrochloric acid and dissolved therein by heating to 40 to 50° C. At 50° C., 25 mL aqueous solution containing 10.3 g of sodium acetate was added dropwise thereto. pH of the reaction mixture was 4.0. After the dropwise addition was completed, the reaction solution was cooled to room temperature and stirred for 1 hour. The crystal was collected by filtration and then washed with a mixture liquid containing 10 mL of acetone and 20 mL of water followed by 30 mL of acetone to obtain 6.1 g of 5-hydroxy-1H-imidazole-4-carboxamide.3/4 hydrate as a gray crystal. The infrared absorption spectrum (ATR method) corresponds to that of Example 4.

후처리

  1. dissolutiondissolved
  2. additionwas added dropwise
  3. additionAfter the dropwise addition
  4. temperaturethe reaction solution was cooled to room temperature
  5. filtrationThe crystal was collected by filtration
  6. washwashed with a mixture liquid
  7. additioncontaining 10 mL of acetone and 20 mL of water

출처 및 근거

ORD 기록
ord-45c8c3cf8d3348f38353dac2cdea7886
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09108928B2

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