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Benzylamine → HCID 14003355、化合物

HRID 1906663
ノート
印刷プレビュー

反応式

HRID 1906663 の反応式
Br[CH2:2][CH2:3][C:4]([NH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:14]([CH3:20])[CH2:15][C:16](=[O:19])[NH:17][N:18]=2)=[CH:9][CH:8]=1)=[O:5].[CH2:21]([NH2:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C(O)CC>[CH2:21]([NH:28][CH2:2][CH2:3][C:4]([NH:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[CH:14]([CH3:20])[CH2:15][C:16](=[O:19])[NH:17][N:18]=2)=[CH:9][CH:8]=1)=[O:5])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7504BenzylamineHCID 140033506-[4-(3-bromopropionamido)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone

生成物 1

HCID 14003355HCID 14003355、化合物収率 88.1%

試薬・触媒・溶媒 1

HCID 10311-Propanol溶媒

実験手順

A suspension of 6-[4-(3-bromopropionamido)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone (120 g, 0.355 mol) and benzylamine (152 g, 1.47 mol) in n-propanol (800 ml) was stirred under reflux for 16 hours. The reaction mixture was filtered whilst hot and white solid was collected, which was washed with ether to remove excess benzylamine. The crude material was boiled with ethanol (300 ml) for 2 hours; the mixture was cooled and filtered. The resulting white solid was washed with ether and dried to give 6-[4-(3-benzylaminopropionamido)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone (114 g, 88%) as the hydrobromide salt m.p. 279°-285° C.

後処理

  1. temperatureunder reflux for 16 hours
  2. filtrationThe reaction mixture was filtered whilst hot and white solid
  3. customwas collected
  4. washwhich was washed with ether
  5. customto remove excess benzylamine
  6. temperaturethe mixture was cooled
  7. filtrationfiltered
  8. washThe resulting white solid was washed with ether
  9. customdried

出典と根拠

ORDレコード
ord-f57a53c01d7a41e3ad12b309cd167aab
出典データセット
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04652563

反応ノート

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