Sodium Methoxide → HCID 12916445, 화합물

HRID 582895노트

반응식

HRID 582895 반응식
Cl[CH:2]([C@H:7]([OH:10])[CH2:8][CH3:9])[C:3]([O:5][CH3:6])=[O:4].C[O-].[Na+]>CO>[O:10]1[C@H:7]([CH2:8][CH3:9])[C@H:2]1[C:3]([O:5][CH3:6])=[O:4]

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 54420244HCID 54420244, 화합물3회

생성물 1

HCID 12916445HCID 12916445, 화합물수율 82.87%

시약·촉매·용매 1

HCID 887Methanol용매3회

실험 절차

To 130 ml of a methanol solution of 25.5 g (0.153 mol) of the methyl (3R)-2-chloro-3-hydroxypentanoate obtained in (2) above was added dropwise 30 g (0.155 mol) of a 28% methanol solution of sodium methoxide at 0 to 5° C., followed by stirring at room temperature for 1 hour. After confirming disappearance of the methyl (3R)-2-chloro-3-hydroxypentanoate by TLC, methanol was evaporated. The concentrate was cooled, adjusted to pH 8 to 9 with 120 ml of a phosphate buffer, and extracted with 300 ml of isopropyl ether. The isopropyl ether was evaporated, and the residue was purified by column chromatography to give 16.5 g (0.126 mol; yield: 82.87%) of the title compound.

후처리

  1. customwas evaporated
  2. temperatureThe concentrate was cooled
  3. extractionextracted with 300 ml of isopropyl ether
  4. customThe isopropyl ether was evaporated
  5. customthe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-5f6971093e0d4e9889f0a5e8d3f9f2e1
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925792

반응 노트

불러오는 중…