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Acetone → Cyclopyrimorate

HRID 1039588
ノート
印刷プレビュー

反応式

HRID 1039588 の反応式
[Cl:1][C:2]1[N:7]=[N:6][C:5]([O:8][C:9]2[C:14]([CH3:15])=[CH:13][CH:12]=[CH:11][C:10]=2[CH:16]2[CH2:18][CH2:17]2)=[C:4]([OH:19])[CH:3]=1.CC(C)=O.C(=O)([O-])[O-].[K+].[K+].[N:30]1([C:36](Cl)=[O:37])[CH2:35][CH2:34][O:33][CH2:32][CH2:31]1>O>[N:30]1([C:36]([O:19][C:4]2[CH:3]=[C:2]([Cl:1])[N:7]=[N:6][C:5]=2[O:8][C:9]2[C:14]([CH3:15])=[CH:13][CH:12]=[CH:11][C:10]=2[CH:16]2[CH2:18][CH2:17]2)=[O:37])[CH2:35][CH2:34][O:33][CH2:32][CH2:31]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 180AcetoneHCID 11430Potassium CarbonateHCID 848104-Morpholinecarbonyl chlorideHCID 178424441HCID 178424441、化合物

生成物 1

HCID 23013854Cyclopyrimorate収率 99.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 19.0 g (68.8 mmol) of 6-chloro-3-(2-cyclopropyl-6-methylphenoxy)-4-pyridazinol were added 51.3 g of acetone and 10.5 g (75.7 mmol) of potassium carbonate, and the resultant mixture was stirred at 30° C. To the mixture was added dropwise 11.3 g (75.7 mmol) of morpholinecarbonyl chloride over one hour. The reaction mixture was subjected to reaction at 30° C. for 5 hours. After completion of the reaction, pure water was added to the reaction mixture to deposit solids, and then the solids were taken out by filtration. The resultant solids were dried under a reduced pressure, and the solids were quantitatively determined by an HPLC internal standard analysis method, which showed that 26.6 g of 6-chloro-3-(2-cyclopropyl-6-methylphenoxy)-4-pyridazinyl morpholine-4-carboxylate (yield: 99%) was obtained.

後処理

  1. customThe reaction mixture was subjected to reaction at 30° C. for 5 hours
  2. additionwas added to the reaction mixture to deposit solids
  3. filtrationthe solids were taken out by filtration
  4. customThe resultant solids were dried under a reduced pressure

出典と根拠

ORDレコード
ord-d2a752ee67d44c63b734f518873b4993
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08552182B2

反応ノート

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