Dichloromethane → HCID 20506149, 화합물

HRID 354760노트

반응식

HRID 354760 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH3:12])[C:10](=[O:13])[C:9]([CH3:15])([CH3:14])[N:8]=[C:7]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[F:22])[C:6]=2[CH:23]=1.Cl.[NH2:25][C:26]([CH3:31])([CH3:30])[C:27](Cl)=[O:28].C(=O)([O-])[O-].[K+].[K+].C(Cl)Cl>O1CCCC1.O>[NH2:25][C:26]([CH3:31])([CH3:30])[C:27]([NH:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH3:12])[C:10](=[O:13])[C:9]([CH3:15])([CH3:14])[N:8]=[C:7]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[F:22])[C:6]=2[CH:23]=1)=[O:28]

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 205061627-amino-5-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-2H-1,4-benzodiazepin-2-oneHCID 214155052-Amino-2-methylpropanoyl chloride hydrochloride

생성물 1

HCID 20506149HCID 20506149, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

8 g (0.026 mol) of 7-amino-5-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-2H-1,4-benzodiazepin-2-one are stirred at room temperature for 1 hour with 5 g of α-aminoisobutyric acid chloride hydrochloride in 30 ml of tetrahydrofuran, 8 g of potassium carbonate are subsequently added thereto and, after a further 15 minutes, the mixture is treated with methylene chloride and water. The organic phase is separated and the aqueous phase is extracted four times with methylene chloride. The combined organic extracts are dried and evaporated. The residue is purified on 350 g of silica gel with methylene chloride/ethyl acetate (1:1) and ethyl acetate as the elution agent. From ethyl acetate/ether there is obtained 2-amino-N-[5-(o-fluorophenyl)-2,3-dihydro-1,3,3-trimethyl-2-oxo-1H-1,4-benzodiazepin-7-yl]-2-methylpropionamide of melting point 250°.

후처리

  1. additionare subsequently added
  2. customThe organic phase is separated
  3. extractionthe aqueous phase is extracted four times with methylene chloride
  4. customThe combined organic extracts are dried
  5. customevaporated
  6. customThe residue is purified on 350 g of silica gel with methylene chloride/ethyl acetate (1:1) and ethyl acetate as the elution agent

출처 및 근거

ORD 기록
ord-11951ee022d94d62a7ce787340d00e77
출처 데이터셋
uspto-grants-1983_03
특허 번호
US04377522

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