Ethyl Acetate → 5-chloro-2-[3-(2-phthalimidoacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone

HRID 614043

반응식

HRID 614043 반응식
[C:1]1(=[O:15])[N:5]([CH2:6][C:7](Cl)=[O:8])[C:4](=[O:10])[C:3]2=[CH:11][CH:12]=[CH:13][CH:14]=[C:2]12.Br.Br.[Cl:18][C:19]1[CH:20]=[CH:21][C:22]([N:33]2[C:37]([CH3:38])=[N:36][N:35]=[C:34]2[CH2:39][NH2:40])=[C:23]([CH:32]=1)[C:24]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:25].C(=O)(O)[O-].[Na+].C(OCC)(=O)C>C1C=CC=CC=1.CN(C)C=O>[Cl:18][C:19]1[CH:20]=[CH:21][C:22]([N:33]2[C:37]([CH3:38])=[N:36][N:35]=[C:34]2[CH2:39][NH:40][C:7](=[O:8])[CH2:6][N:5]2[C:4](=[O:10])[C:3]3=[CH:11][CH:12]=[CH:13][CH:14]=[C:2]3[C:1]2=[O:15])=[C:23]([CH:32]=1)[C:24]([C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1)=[O:25]

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 812422H-Isoindole-2-acetyl chloride, 1,3-dihydro-1,3-dioxo-HCID 516892Sodium BicarbonateHCID 213257365-chloro-2-(3-aminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone dihydrobromide

생성물 1

HCID 155678715-chloro-2-[3-(2-phthalimidoacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone수율 69.4%

시약·촉매·용매 2

HCID 241Benzene용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of 2-phthalimidoacetyl chloride (1.5 g) in benzene (20 ml) and dimethylformamide (10 ml), 5-chloro-2-(3-aminomethyl-5-methyl-4H-1,2,4-triazol-4-yl)-benzophenone dihydrobromide (2.3 g) is added under ice cooling and stirring, and the temperature within the flask is gradually returned to room temperature. The reaction mixture is allowed to stand at room temperature, neutralized with saturated aqueous sodium bicarbonate, and shaken with ethyl acetate. The precipitated crystals are filtered, washed with methanol and dried to give 5-chloro-2-[3-(2-phthalimidoacetamidomethyl)-5-methyl-4H-1,2,4-triazol-4-yl]-benzophenone (1.68 g) as crystals melting at 251°-253° C.

후처리

  1. customis gradually returned to room temperature
  2. customto stand at room temperature
  3. filtrationThe precipitated crystals are filtered
  4. washwashed with methanol
  5. customdried

출처 및 근거

ORD 기록
ord-7b823883da4a4fdf95457f201a2c32df
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04143048

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