N-Hydroxypropionimidamide → HCID 22318613、化合物

HRID 497048ノート

反応式

HRID 497048 の反応式
[Cl:1][C:2]1[C:3]([O:18][CH2:19][CH2:20][CH2:21][O:22][C:23]2[CH:28]=[CH:27][C:26]([C:29]([F:32])([F:31])[F:30])=[CH:25][N:24]=2)=[C:4]([CH:9]=[C:10]([O:12][CH2:13][CH:14]=[C:15]([Cl:17])[Cl:16])[CH:11]=1)[C:5](OC)=[O:6].[C:33](=[N:37]O)([NH2:36])[CH2:34][CH3:35].[Na]>C(O)C>[Cl:1][C:2]1[CH:11]=[C:10]([O:12][CH2:13][CH:14]=[C:15]([Cl:17])[Cl:16])[CH:9]=[C:4]([C:5]2[O:6][N:37]=[C:33]([CH2:34][CH3:35])[N:36]=2)[C:3]=1[O:18][CH2:19][CH2:20][CH2:21][O:22][C:23]1[CH:28]=[CH:27][C:26]([C:29]([F:30])([F:31])[F:32])=[CH:25][N:24]=1

参加物

5

反応物 3

HCID 4092053N-HydroxypropionimidamideHCID 5360545SodiumHCID 22318619HCID 22318619、化合物

生成物 1

HCID 22318613HCID 22318613、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
40 °C

実験手順

0.05 g of methyl 3-chloro-5-(3,3-dichloroprop-2-enyloxy)-2-[3-(5-trifluoromethylpyrid-2-yloxy)propyloxy]benzoate and 0.028 g of propionamidoxime were dissolved in 1 ml of anhydrous ethanol. A solution of 0.008 g of sodium in 0.5 ml of ethanol was added to this solution. The mixture was stirred at 40° C. for 2 hours and at room temperature for 20 hours. The mixture was then concentrated, and diethyl ether and water were added. After shaking, the ether phase was isolated, dried and concentrated under reduced pressure, and the crude product was purified chromatographically. Yield: 0.017 g (32%)

後処理

  1. concentrationThe mixture was then concentrated
  2. additiondiethyl ether and water were added
  3. stirringAfter shaking
  4. customthe ether phase was isolated
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customthe crude product was purified chromatographically

出典と根拠

ORDレコード
ord-68ae83fbb67c491bb414b7c859e79a24
出典データセット
uspto-grants-2005_09
特許番号
US06949551B2

反応ノート

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