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Toluene → Cyclopyrimorate

HRID 1039589
ノート
印刷プレビュー

反応式

HRID 1039589 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.C1(C)C=CC=CC=1.C(N(CC)CC)C.[N:34]1([C:40](Cl)=[O:41])[CH2:39][CH2:38][O:37][CH2:36][CH2:35]1>O>[N:34]1([C:40]([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:41])[CH2:39][CH2:38][O:37][CH2:36][CH2:35]1
参加物反応条件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 1140TolueneHCID 8471TriethylamineHCID 848104-Morpholinecarbonyl chlorideHCID 178424441HCID 178424441、化合物

生成物 1

HCID 23013854Cyclopyrimorate収率 99%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

To 6.50 g (23.5 mmol) of 6-chloro-3-(2-cyclopropyl-6-methylphenoxy)-4-pyridazinol were added 39 g of toluene and 2.62 g (25.9 mmol) of triethylamine, and the resultant mixture was stirred at 30° C. To the mixture was added dropwise 7.73 g (51.7 mmol) of morpholinecarbonyl chloride over one hour. The reaction mixture was subjected to reaction at 30° C. for 2 hours, and then further heated to 50° C. to effect a reaction for 2 hours. After completion of the reaction, pure water was added to the reaction mixture, and an organic phase and an aqueous phase were separated, and then the resultant organic phase was quantitatively determined by an HPLC internal standard analysis method, which showed that 9.07 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 2 hours
  2. customa reaction for 2 hours
  3. additionwas added to the reaction mixture
  4. customan organic phase and an aqueous phase were separated

出典と根拠

ORDレコード
ord-2a0c06bd7b6b453fb08434bd052bb506
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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