Hydrochloric Acid → HCID 178513824、化合物

HRID 514676ノート

反応式

HRID 514676 の反応式
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.[Na+]>>[OH:4][C:5]1[NH:9][CH:8]=[N:7][C:6]=1[C:10]([NH2:12])=[O:11]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 2723810Sodium FormateHCID 178479550HCID 178479550、化合物

生成物 1

HCID 178513824HCID 178513824、化合物収率 98.9%

反応条件

温度
50 °C

実験手順

Under the nitrogen atmosphere, 20.0 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate prepared according to the method of Reference Example 2 was added to 240 mL of 0.45 mol/L hydrochloric acid and dissolved therein by heating to 50° C. At 50° C., 40 mL aqueous solution containing 14.3 g of sodium formate was added dropwise thereto over 35 minutes. The reaction mixture was cooled and stirred for 90 minutes with the inside temperature of 5° C. The crystal was collected by filtration and then washed with a mixture liquid containing 20 mL of acetone and 40 mL of water followed by 60 mL of acetone to give 12.6 g of 5-hydroxy-1H-imidazole-4-carboxamide.3/4 hydrate as a pale yellow crystal.

後処理

  1. dissolutiondissolved
  2. additionwas added dropwise
  3. temperatureThe reaction mixture was cooled
  4. filtrationThe crystal was collected by filtration
  5. washwashed with a mixture liquid
  6. additioncontaining 20 mL of acetone and 40 mL of water

出典と根拠

ORDレコード
ord-7a26519181884950b0d8142ed4d3f191
出典データセット
uspto-grants-2015_08
特許番号
US09108928B2

反応ノート

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