Hydrochloric Acid → HCID 6713300, 화합물

HRID 990569노트

반응식

HRID 990569 반응식
Cl.[CH3:2][C:3]([CH3:9])([C:5](=[O:8])[CH2:6][CH3:7])[CH3:4].[N:10](OCCCC)=[O:11]>C(OCC)C.C1(C)C=CC=CC=1>[OH:11][N:10]=[C:6]([CH3:7])[C:5](=[O:8])[C:3]([CH3:9])([CH3:4])[CH3:2]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 10996Butyl nitriteHCID 1363632,2-Dimethyl-3-pentanone

생성물 1

HCID 6713300HCID 6713300, 화합물수율 55%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3283Diethyl Ether용매2회

반응 조건

온도
-10 °C

실험 절차

A solution of 40 g of hydrogen chloride in 156 g of diethyl ether is added dropwise at room temperature to 96 g (0.84 mol) of 2,2-dimethyl-3-pentanone in 960 g of toluene. After cooling to −10° C., a solution of 95g of n-butyl nitrite in 470 g of diethyl ether is added dropwise. The mixture is stirred at from −10° C. to 0° C. for 4 hours and then allowed to come to room temperature. After a total of 16 h, the reaction mixture is washed three times with 1 l of ice-water each time and then extracted twice with 1 l of 1M sodium hydroxide solution each time. The alkaline phase is separated off and neutralized with 20% strength sulfuric acid. The crude product is filtered off with suction and, after drying, recrystallized from n-hexane. 66 g (55%) of the title compound are obtained as a pale yellow powder of melting point 107-110° C.

후처리

  1. customto come to room temperature
  2. washAfter a total of 16 h, the reaction mixture is washed three times with 1 l of ice-water each time
  3. extractionextracted twice with 1 l of 1M sodium hydroxide solution each time
  4. customThe alkaline phase is separated off
  5. filtrationThe crude product is filtered off with suction
  6. customafter drying
  7. customrecrystallized from n-hexane

출처 및 근거

ORD 기록
ord-f873d515bbc548a781477f7c777adae8
출처 데이터셋
uspto-grants-2002_10
특허 번호
USRE037873E1

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