Acetyl chloride → HCID 85826160, 화합물

HRID 2064673노트

반응식

HRID 2064673 반응식
[Cl-].[Mg+2].[Cl-].[CH2:4]([O:6][C:7](=[O:17])[CH2:8][C:9](=[O:16])[CH2:10][O:11][C:12]([CH3:15])([CH3:14])[CH3:13])[CH3:5].[C:18](Cl)(=[O:20])[CH3:19].[Cl-].[NH4+]>ClCCl.N1C=CC=CC=1>[CH2:4]([O:6][C:7](=[O:17])[CH:8]([C:18](=[O:20])[CH3:19])[C:9](=[O:16])[CH2:10][O:11][C:12]([CH3:13])([CH3:15])[CH3:14])[CH3:5]

참가 물질

7

반응물 4

HCID 6367Acetyl chlorideHCID 25517Ammonium ChlorideHCID 5360315Magnesium ChlorideHCID 11790264Ethyl 4-(tert-butoxy)-3-oxobutanoate

생성물 1

HCID 85826160HCID 85826160, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

A suspension of dry magnesium chloride (0.471 g) in dichloromethane (6 ml) was treated with 4-tert-butoxy-3-oxo-butyric acid ethyl ester [1.00 g, Reference Example 43]. This mixture was cooled to 0° C., then treated with pyridine (0.80 ml), then stirred for 15 minutes at 0° C. and then treated with acetyl chloride (0.352 ml). After stirring for a further 15 minutes at 0° C. and then for 1 hour at ambient temperature the reaction mixture was treated with saturated aqueous ammonium chloride solution and then extracted twice with ethyl acetate. The combined extracts were dried over magnesium sulfate and then evaporated to yield 2-acetyl-4-tert-butoxy-3-oxo-butyric acid ethyl ester (1.15 g) as a yellow oil which was used without further purification. LC-MS (METHOD B): RT=3.16 minutes; 243 (M−H)−.

후처리

  1. stirringAfter stirring for a further 15 minutes at 0° C.
  2. extractionextracted twice with ethyl acetate
  3. dry with materialThe combined extracts were dried over magnesium sulfate
  4. customevaporated

출처 및 근거

ORD 기록
ord-911552e7b9464f0991adb0a205215e01
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288425B2

반응 노트

불러오는 중…