Malonic Acid → HCID 14848100、化合物

HRID 1199745ノート

反応式

HRID 1199745 の反応式
[CH2:1]([NH:5][C:6]([NH:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)=[O:7])[CH2:2][CH2:3][CH3:4].[C:15](O)(=[O:20])[CH2:16][C:17](O)=[O:18].C(OC(=O)C)(=O)C>C(O)(=O)C>[CH2:1]([N:5]1[C:15](=[O:20])[CH2:16][C:17](=[O:18])[N:8]([CH:9]2[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]2)[C:6]1=[O:7])[CH2:2][CH2:3][CH3:4]

参加物

5

反応物 3

HCID 867Malonic AcidHCID 7918Acetic AnhydrideHCID 36136763-butyl-1-cyclohexylurea

生成物 1

HCID 14848100HCID 14848100、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
60 °C

実験手順

A solution was prepared by adding 15.87 gm (0.080 mole) of 1-(1-butyl)-3-cyclohexylurea and 8.33 gm (0.080 mole) of malonic acid to 35 mL of reagent grade acetic acid in a 250 mL 3-neck, round bottom flask equipped with a thermometer, pressure equalizing dropping funnel capped by a drying tube, nitrogen inlet and magnetic stirrer. The stirred mixture was gradually heated to 60° C. in a silicone oil bath. All of the solid dissolved before the temperature reached 60° C. A total of 32 mL of acetic anhydride was added to the dropping funnel and slowly (over a period of about 45 min.) dropped into the stirred reaction flask. The temperature was gradually increased to approximately 90° C. for 7 hours, then allowed to cool to room temperature and stand overnight.

後処理

  1. customA solution was prepared
  2. customequipped with a thermometer, pressure
  3. customcapped by a drying tube, nitrogen inlet and magnetic stirrer
  4. dissolutionAll of the solid dissolved before the temperature
  5. customreached 60° C
  6. additionslowly (over a period of about 45 min.) dropped into the stirred reaction flask
  7. temperatureThe temperature was gradually increased to approximately 90° C. for 7 hours
  8. temperatureto cool to room temperature

出典と根拠

ORDレコード
ord-60525b11f060441c9383e4e586c10abf
出典データセット
uspto-grants-1990_02
特許番号
US04902784

反応ノート

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