Sodium Hydroxide → 1-(4-Carboxybenzyl)-4-(4-chlorobenzoyl)-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on

HRID 2417473노트

반응식

HRID 2417473 반응식
[Cl:1][C:2]1[CH:21]=[CH:20][C:5]([C:6]([N:8]2[CH2:14][C:13]3[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=3[NH:11][C:10](=[O:19])[CH2:9]2)=[O:7])=[CH:4][CH:3]=1.[H-].[Na+].Br[CH2:25][C:26]1[CH:35]=[CH:34][C:29]([C:30]([O:32]C)=[O:31])=[CH:28][CH:27]=1.[OH-].[Na+]>CN(C=O)C.C(OCC)(=O)C.C(O)C.C1COCC1>[C:30]([C:29]1[CH:34]=[CH:35][C:26]([CH2:25][N:11]2[C:12]3[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=3[CH2:14][N:8]([C:6](=[O:7])[C:5]3[CH:20]=[CH:21][C:2]([Cl:1])=[CH:3][CH:4]=3)[CH2:9][C:10]2=[O:19])=[CH:27][CH:28]=1)([OH:32])=[O:31]

참가 물질

9

반응물 4

HCID 14798Sodium HydroxideHCID 24758Sodium hydrideHCID 256687Methyl 4-(bromomethyl)benzoateHCID 226325544-(4-Chlorobenzoyl)-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on

생성물 1

HCID 226325341-(4-Carboxybenzyl)-4-(4-chlorobenzoyl)-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on

시약·촉매·용매 4

HCID 702Ethanol용매HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매2회

실험 절차

300 mg (1.0 mmol) of 4-(4-chlorobenzoyl)-1,3,4,5-tetrahydrobenzo[e][1,4]diazepin-2-on was dissolved in 10 ml of DMF. 48 mg (1.2 mmol) of sodium hydride was added to the obtained solution, and they were stirred at room temperature for 30 minutes. 300 mg (1.3 mmol) of methyl 4-bromomethylbenzoate was added to the obtained mixture, and they were stirred at 60° C. overnight. After the treatment with ethyl acetate as the extracting solvent, the obtained crude product was stirred together with 2 ml of THF, 2 ml of ethanol and 2 ml of 1 N aqueous sodium hydroxide solution at room temperature overnight. The obtained product was treated with ethyl acetate as the extracting solvent by an ordinary method to obtain the crude product.

후처리

  1. stirringwere stirred at 60° C. overnight

출처 및 근거

ORD 기록
ord-205b1ef72a194d9693dacd493e87f40b
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06825191B2

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