Triethylamine → 5-Ethoxycarbonyl-2-methoxy-2-oxo-1,3,2-benzo-dioxaphosphole

HRID 2292384

반응식

HRID 2292384 반응식
C(N(CC)CC)C.[OH:8][C:9]1[CH:10]=[C:11]([CH:17]=[CH:18][C:19]=1[OH:20])[C:12]([O:14][CH2:15][CH3:16])=[O:13].[P:21](Cl)(Cl)([O:23][CH3:24])=[O:22]>CCOCC>[CH2:15]([O:14][C:12]([C:11]1[CH:17]=[CH:18][C:19]2[O:20][P:21]([O:23][CH3:24])(=[O:22])[O:8][C:9]=2[CH:10]=1)=[O:13])[CH3:16]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 69611Methyl dichlorophosphateHCID 77547Ethyl 3,4-Dihydroxybenzoate

생성물 1

HCID 200765455-Ethoxycarbonyl-2-methoxy-2-oxo-1,3,2-benzo-dioxaphosphole수율 84.7%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

Triethylamine (2.211 g, 21.86 mM) was added to a solution of 1.989 g (10.93 mM) of ethyl 3,4-dihydroxybenzoate in 30 ml of ether. The mixture was cooled to -30° C. to -20° C. and a solution of 1.627 g (10.93 mM) of methyl dichlorophosphate in 10 ml of ether was added thereto dropwise with stirring over 10 minutes. The reaction mixture was stirred at the same temperature for 5 minutes, the bath was then removed and the temperature was allowed to rise to 20° C. Filtration and washing were carried out by the procedure of Reference Example 1, and the filtrate and washings were concentrated at room temperature (20°~25° C.) under reduced pressure. There was obtained 2.387 g (84.6% yield) of 5-ethoxycarbonyl-2-methoxy-2-oxo-1,3,2-benzo-dioxaphosphole as a viscous oil.

후처리

  1. temperatureThe mixture was cooled to -30° C. to -20° C.
  2. stirringThe reaction mixture was stirred at the same temperature for 5 minutes
  3. customthe bath was then removed
  4. customto rise to 20° C
  5. filtrationFiltration
  6. washwashing
  7. concentrationthe filtrate and washings were concentrated at room temperature (20°~25° C.) under reduced pressure

출처 및 근거

ORD 기록
ord-cabb5ab605c64d3ea3581d183779e73e
출처 데이터셋
uspto-grants-1989_01
특허 번호
US04801703

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