Boron trifluoride etherate → Methyl 3-ethoxy-2-(ethoxyimino)-3-iminopropanoate

HRID 1247918

反応式

HRID 1247918 の反応式
F[B-](F)(F)F.[CH2:6]([O+](CC)CC)[CH3:7].B(F)(F)F.CCOCC.[C:22]([C:25](=[N:30][O:31][CH2:32][CH3:33])[C:26]([O:28][CH3:29])=[O:27])(=[O:24])[NH2:23].C(N(CC)CC)C>C(Cl)Cl.O>[NH:23]=[C:22]([O:24][CH2:6][CH3:7])[C:25](=[N:30][O:31][CH2:32][CH3:33])[C:26]([O:28][CH3:29])=[O:27]

参加物

7

反応物 4

HCID 8000Boron trifluoride etherateHCID 8471TriethylamineHCID 2723982Triethyloxonium tetrafluoroborateHCID 53690437Methyl 3-amino-2-(ethoxyimino)-3-oxopropanoate

生成物 1

HCID 53663360Methyl 3-ethoxy-2-(ethoxyimino)-3-iminopropanoate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of Meerwein reagent (triethyloxonium tetrafluoroborate) {prepared from boron fluoride etherate (2.84 g) by a method of Org. Syn., 46, 113 (1966)} in methylene chloride (30 ml) was added methyl 2-carbamoyl-2-ethoxyiminoacetate (syn isomer, 2.6 g) and the mixture was stirred for 18 hours at room temperature. The reaction mixture was cooled in an ice-bath and triethylamine (3 g) was added thereto, followed by an addition of water (20 ml). The organic layer was separated out, dried over magnesium sulfate and evaporated to give crude methyl 3-imino-3-ethoxy-2-ethoxyiminopropionate (syn isomer) (5.0 g) as an oil. ##STR14##

後処理

  1. temperatureThe reaction mixture was cooled in an ice-bath
  2. customThe organic layer was separated out
  3. dry with materialdried over magnesium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-ce94f06b2c1b4a598fdad22af5a00bbe
出典データセット
uspto-grants-1985_06
特許番号
US04521413

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