Hydrochloric Acid → HCID 178516753、化合物

HRID 2060250

反応式

HRID 2060250 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH:9]=O)=[CH:4][CH:3]=1.[NH2:12][CH2:13][C:14]([NH2:16])=[O:15].[OH-].[Na+].Cl.C(=O)(O)[O-].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:12]=[CH:13][C:14]([OH:15])=[N:16][CH:9]=2)=[CH:6][CH:7]=1

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 69020GlycinamideHCID 269588(4-Chlorophenyl)(oxo)acetaldehydeHCID 516892Sodium Bicarbonate

生成物 1

HCID 178516753HCID 178516753、化合物収率 37.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
-30 °C

実験手順

To a stirred solution of (4-chloro-phenyl)-oxo-acetaldehyde (300 mg, 1.69 mmol) in methanol (15 mL) was added 2-amino-acetamide (187 mg, 1.69 mmol). The resulting mixture was cooled to −30° C. and 12.5M aqueous sodium hydroxide solution (0.3 mL) added. The resulting mixture was allowed to warm to −5° C. and was stirred at this temperature for 2 hours, followed by stirring at room temperature for 2 hours. Concentrated aqueous hydrogen chloride (0.3 mL) was added, followed by saturated sodium bicarbonate solution (1.0 mL). The reaction mixture was filtered and the resulting solid was washed with water (10 mL) and dried in a vacuum oven to afford the title compound as a brown solid (130 mg, 37%)

後処理

  1. temperatureto warm to −5° C.
  2. stirringby stirring at room temperature for 2 hours
  3. filtrationThe reaction mixture was filtered
  4. washthe resulting solid was washed with water (10 mL)
  5. customdried in a vacuum oven

出典と根拠

ORDレコード
ord-bacc7dfb8db14fada60bd2545ce4e55c
出典データセット
uspto-grants-2012_10
特許番号
US08278343B2

関連ノート

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