Dichloromethane → HCID 178472018、化合物

HRID 1608353

反応式

HRID 1608353 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 178472018HCID 178472018、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bc334eff4b694b77b9c6c52b73680e71
出典データセット
uspto-grants-1989_09
特許番号
US04870182

関連ノート

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