Hydrochloric Acid → HCID 178513824, 화합물

HRID 514680

반응식

HRID 514680 반응식
O.O.Cl.[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11].Cl.C([O-])(=O)C(CC([O-])=O)O.[Na+].[Na+]>>[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 8736Malic acid, disodium saltHCID 178479550HCID 178479550, 화합물

생성물 1

HCID 178513824HCID 178513824, 화합물수율 93.2%

반응 조건

온도
50 °C

실험 절차

Under the nitrogen atmosphere, 1.5 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate prepared according to the method of Reference Example 2 was added to 18 mL of 0.45 mol/L hydrochloric acid and dissolved therein by heating to 50° C. At 50° C., 6 mL aqueous solution containing 3.5 g of sodium malate was added dropwise thereto. pH of the reaction mixture was 2.6. The reaction mixture was cooled to room temperature. The crystal was collected by filtration and then washed with a mixture liquid containing 1.5 mL of acetone and 3.0 mL of water followed by 4.5 mL of acetone to give 0.89 g of 5-hydroxy-1H-imidazole-4-carboxamide.3/4 hydrate as a pale yellow crystal. The infrared absorption spectrum (ATR method) corresponds to that of Example 4.

후처리

  1. dissolutiondissolved
  2. additionwas added dropwise
  3. temperatureThe reaction mixture was cooled to room temperature
  4. filtrationThe crystal was collected by filtration
  5. washwashed with a mixture liquid
  6. additioncontaining 1.5 mL of acetone and 3.0 mL of water

출처 및 근거

ORD 기록
ord-7e10318896534e01932dbefdd8bdcc6e
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09108928B2

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