Dichloromethane → HCID 178472018, 화합물

HRID 1608353

반응식

HRID 1608353 반응식
[Cl:1][C:2]1[C:19]([N+:20]([O-:22])=[O:21])=[C:18]([Cl:23])[C:17]([F:24])=[CH:16][C:3]=1[C:4]([C:6](=[CH:12]OCC)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5].C(Cl)Cl.Cl.[NH2:29][CH2:30][CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33].C([O-])(O)=O.[Na+]>O>[Cl:1][C:2]1[C:19]([N+:20]([O-:22])=[O:21])=[C:18]([Cl:23])[C:17]([F:24])=[CH:16][C:3]=1[C:4]([C:6](=[CH:12][NH:29][CH2:30][CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 458475beta-Alanine, ethyl ester, hydrochlorideHCID 516892Sodium BicarbonateHCID 53944414Ethyl 2-(2,4-dichloro-5-fluoro-3-nitrobenzoyl)-3-ethoxyacrylate

생성물 1

HCID 178472018HCID 178472018, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

38 g of ethoxy acrylate from Example 1 are initially introduced into 150 ml of methylene chloride. An aqueous solution of 15.4 g of ethyl 3-aminopropionate hydrochloride is added to this. A solution of 8.4 g of NaHCO3 in water is added dropwise to the two-phase system with vigorous stirring. After completion of the dropwise addition, the mixture is stirred for a further 2 hours, and the phases are subsequently separated. The organic phase is washed with water, dried over Na2SO4, and concentrated. The solid residue is slurried in diethyl ether and subsequently isolated. Yield: 38 g, melting point 107°-8° C.

후처리

  1. additionAfter completion of the dropwise addition
  2. customthe phases are subsequently separated
  3. washThe organic phase is washed with water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. customsubsequently isolated

출처 및 근거

ORD 기록
ord-bc334eff4b694b77b9c6c52b73680e71
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04870182

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