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

HRID 1247918
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HRID 1247918 반응식
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]
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참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water
용매
HCID 6344Dichloromethane용매

실험 절차

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##

후처리

  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

출처 및 근거

ORD 기록
ord-ce94f06b2c1b4a598fdad22af5a00bbe
출처 데이터셋
uspto-grants-1985_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04521413

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