5-chloro-2-(3-carbobenzoxyaminomethyl-5-chloromethyl-4H-1,2,4-triazol-4-yl)-benzophenone → 5-chloro-2-(3-acetamidomethyl-5-chloromethyl-4H-1,2,4-triazol-4-yl)-benzophenone

HRID 25945

反応式

HRID 25945 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:16]2[C:20]([CH2:21][Cl:22])=[N:19][N:18]=[C:17]2[CH2:23][NH:24][C:25]([O:27]CC2C=CC=CC=2)=O)=[C:6]([CH:15]=1)[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:8].Br.[C:36](O)(=O)C>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:16]2[C:20]([CH2:21][Cl:22])=[N:19][N:18]=[C:17]2[CH2:23][NH:24][C:25](=[O:27])[CH3:36])=[C:6]([CH:15]=1)[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:8]

参加物

3

反応物 2

HCID 213257095-chloro-2-(3-carbobenzoxyaminomethyl-5-chloromethyl-4H-1,2,4-triazol-4-yl)-benzophenoneHCID 21893785Acetic Acid Mixture with Hydrobromic Acid

生成物 1

HCID 213256895-chloro-2-(3-acetamidomethyl-5-chloromethyl-4H-1,2,4-triazol-4-yl)-benzophenone

実験手順

A mixture of 5-chloro-2-[3-(N-carbobenzoxyaminomethyl)-5-chloromethyl-4H-1,2,4-triazol-4-yl]-benzophenone (0.995 g) and 30% hydrogen bromide-acetic acid (2 ml) is stirred at room temperature for 1.25 hours, and the mixture is washed with ether (50 ml) twice. The obtained free base is mixed with benzene (10 ml), acetyl chloride (0.5 g) and dimethylformamide (6 ml), and the resultant mixture is stirred at room temperature for 2 hours, and allowed to stand overnight. The reaction mixture is neutralized with aqueous sodium bicarbonate, and the precipitated crystals are filtered and washed with ether and chloroform in order to give 5-chloro-2-(3-acetamidomethyl-5-chloromethyl-4H-1,2,4-triazol-4-yl)-benzophenone (0.6 g) as crystals melting at 193° to 199° C. (decomp.).

後処理

  1. washthe mixture is washed with ether (50 ml) twice
  2. additionThe obtained free base is mixed with benzene (10 ml), acetyl chloride (0.5 g) and dimethylformamide (6 ml)
  3. stirringthe resultant mixture is stirred at room temperature for 2 hours
  4. waitto stand overnight
  5. filtrationthe precipitated crystals are filtered
  6. washwashed with ether and chloroform in order

出典と根拠

ORDレコード
ord-8a125b234fb749b196711dc59ecc4c9e
出典データセット
uspto-grants-1979_04
特許番号
US04147700

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