Hydrochloric Acid → Ethyl (chloroformyl)acetate

HRID 53924

반응식

HRID 53924 반응식
C[C:2](C)([O-:4])C.[K+].[Cl:7][CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10].C(OCC)=O.Cl>C1COCC1.C(OCC)C>[Cl:7][CH:8]([CH:2]=[O:4])[C:9]([O:11][CH2:12][CH3:13])=[O:10]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 7751Ethyl chloroacetateHCID 8025Ethyl formateHCID 23665647Potassium tert-butoxide

생성물 1

HCID 118030Ethyl (chloroformyl)acetate

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매3회

반응 조건

온도
0 °C

실험 절차

To a three neck 2 L round bottom flask charged with potassium t-butoxide (0.5 mol, 500 mL of a 1M solution in THF) and 500 mL of dry THF cooled to 0° C. was added dropwise from an addition funnel a solution of ethyl chloroacetate (0.5 mol, 53.5 mL) and ethyl formate (0.5 mol, 40.4 mL), in 200 mL of THF over 3 hours. After completion of addition, the reaction mixture was stirred for 1 hour and allowed to stand overnight. The resulting solid was diluted with diethyl ether and cooled in an ice bath. Then, the pH was lowered to approximately 3 using 6N HCl. The organic phase was separated, and the aqueous layer was washed 3 times with diethyl ether. The combined ethereal portions were dried over NaSO4, and concentrated in vacuo. The crude desired compound was stored at -30° C. and used without further purification.

후처리

  1. additionAfter completion of addition
  2. waitto stand overnight
  3. temperaturecooled in an ice bath
  4. customThe organic phase was separated
  5. washthe aqueous layer was washed 3 times with diethyl ether
  6. dry with materialThe combined ethereal portions were dried over NaSO4
  7. concentrationconcentrated in vacuo
  8. customwas stored at -30° C.
  9. customused without further purification

출처 및 근거

ORD 기록
ord-24a572f086054e7eacbff4c2c637f301
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05621109

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