Hydrochloric Acid → HCID 178518769、化合物

HRID 274462

反応式

HRID 274462 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([C:12](=O)[C:13]([O:15]CCCCCC)=O)[CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[C:7]=1[OH:8].[NH2:23][NH:24][C:25]([NH2:27])=[S:26].[OH-].[Na+].Cl>O>[OH:1][C:2]1[CH:3]=[C:4]([C:12]2[C:13](=[O:15])[NH:27][C:25]([SH:26])=[N:24][N:23]=2)[CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[C:7]=1[OH:8]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 2723789ThiosemicarbazideHCID 5747978Benzeneacetic acid, 3,4-dihydroxy-5-nitro-alpha-oxo-, hexyl ester

生成物 1

HCID 178518769HCID 178518769、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A suspension of 2.05 g of n-hexyl 3,4-dihydroxy-5-nitrophenylglyoxylate and 600.8 mg of thiosemicarbazide is stirred intensively at 90° for 30 minutes. The mixture is then cooled to 40° and treated with a solution of 870.1 mg of sodium hydroxide in 15 ml of water. The solution is subsequently heated to 90° for 30 minutes, cooled to room temperature and treated dropwise with 2 ml of conc. hydrochloric acid. The crystallized-out product is filtered under suction and then dissolved in ethyl acetate. The solution is washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and evaporated. There is obtained 6-(3,4-dihydroxy-5-nitrophenyl)-3 -mercapto-1,2,4-triazin-5(4H)-one of m.p. 282°-284° (from ethanol).

後処理

  1. temperatureThe mixture is then cooled to 40°
  2. temperatureThe solution is subsequently heated to 90° for 30 minutes
  3. filtrationThe crystallized-out product is filtered under suction
  4. dissolutiondissolved in ethyl acetate
  5. washThe solution is washed with saturated sodium chloride solution
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated

出典と根拠

ORDレコード
ord-0a995d9310f74590883bc686e2fc90c0
出典データセット
uspto-grants-1995_02
特許番号
US05389653

関連ノート

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