Dimethylamine → N,N-Dimethyl-2,3-dihydro-3-oxo-5,6-diphenyl-4-pyridazinecarboxamide

HRID 463965ノート

反応式

HRID 463965 の反応式
[C:1]([C:4]1[C:5](=[O:22])[NH:6][N:7]=[C:8]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:9]=1[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(O)=[O:2].[CH3:23][NH:24][CH3:25]>C1(C)C=CC=CC=1>[CH3:23][N:24]([CH3:25])[C:1]([C:4]1[C:5](=[O:22])[NH:6][N:7]=[C:8]([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:9]=1[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[O:2]

参加物

4

反応物 2

HCID 674DimethylamineHCID 735030F3099-5022

生成物 1

HCID 13533378N,N-Dimethyl-2,3-dihydro-3-oxo-5,6-diphenyl-4-pyridazinecarboxamide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

8.0 grams (0.0275 mole) of the acid chloride of the product of Example 2 was reacted with excess dimethylamine in 200 mls of toluene. This solution was heated on a steam bath for 2 hours. The solution was filtered and the filtrate distilled at reduced pressure. The residual solid was filtered, washed with petroleum ether and air dried. There was isolated 5.0 grams of a solid which when recrystallized from absolute ethyl alcohol gave 2.5 grams of a white solid that melted at 278° C. The infrared spectrum showed two carbonyl bands one at 6.0μ, the other a 6.1μ. Analysis calculated for C19H17N3O2.1H2O, C, 70.4; H, 5.4; N, 12.9. Found: C, 70.1; H, 5.5; N, 12.9.

後処理

  1. temperatureThis solution was heated on a steam bath for 2 hours
  2. filtrationThe solution was filtered
  3. distillationthe filtrate distilled at reduced pressure
  4. filtrationThe residual solid was filtered
  5. washwashed with petroleum ether and air
  6. customdried

出典と根拠

ORDレコード
ord-8b6839e90a63456e9b55cccb1f6c26b4
出典データセット
uspto-grants-1985_10
特許番号
US04545810

反応ノート

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