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

반응식

HRID 25945 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-8a125b234fb749b196711dc59ecc4c9e
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04147700

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