Water → HCID 13084131、化合物

HRID 67266

反応式

HRID 67266 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:13]([CH3:14])=[CH:12][C:11](=[O:15])[C:10]([C:16]([OH:18])=O)=[N:9]2)=[CH:4][CH:3]=1.C(N(CC)CC)C.[CH2:26]([NH:30][CH2:31][CH2:32][CH2:33][CH3:34])[CH2:27][CH2:28][CH3:29].O>C1(C)C=CC=CC=1>[CH2:26]([N:30]([CH2:31][CH2:32][CH2:33][CH3:34])[C:16]([C:10]1[C:11](=[O:15])[CH:12]=[C:13]([CH3:14])[N:8]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)[N:9]=1)=[O:18])[CH2:27][CH2:28][CH3:29]

参加物

6

反応物 4

HCID 962WaterHCID 8148DibutylamineHCID 8471TriethylamineHCID 197225Fenridazon

生成物 1

HCID 13084131HCID 13084131、化合物収率 73.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

To an ice cooled suspension of 5.29 g (0.02 mol) 1-(4-chlorophenyl)-1,4-dihydro-4-oxo-6-methyl pyridazine-3-carboxylic Acid (see Example 12) and 2.02 g (0.02 mol) of triethylamine in 100 ml of toluene there is added dropwise 2.17 g (0.02 mol) of ethyl chlorofomate. The suspension formed is stirred at room temperature for 15 min. and is cooled to 5° C. To the suspension is added 2.59 g (0.02 mol) di-n-butylamine and the mixture is stirred at room temperature for 18 hrs. To the mixture is added 100 ml of water and the suspension formed is stirred at room temperature for 1 hr. The toluene layer is isolated, dried over magnesium sulfate and concentrated in vacuo. The residue oil is dissolved in 25 ml of ether and to it there is added 25 ml of hexane. The mixture is allowed to stand at room temperature for 30 minutes and is vacuum filtered. The filter cake is washed with hexane and air dried to afford 5.5 g (73% yield) of product, mp 101°-105° C.

後処理

  1. additionthere is added dropwise 2.17 g (0.02 mol) of ethyl chlorofomate
  2. customThe suspension formed
  3. temperatureis cooled to 5° C
  4. stirringthe mixture is stirred at room temperature for 18 hrs
  5. customthe suspension formed
  6. stirringis stirred at room temperature for 1 hr
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated in vacuo
  9. dissolutionThe residue oil is dissolved in 25 ml of ether and to it there
  10. additionis added 25 ml of hexane
  11. waitto stand at room temperature for 30 minutes
  12. filtrationfiltered
  13. washThe filter cake is washed with hexane and air
  14. customdried

出典と根拠

ORDレコード
ord-adeb08de34bc457090a8057060728236
出典データセット
uspto-grants-1982_08
特許番号
US04345934

関連ノート

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