Sodium Chloride → HCID 12014811, 화합물

HRID 1585165노트

반응식

HRID 1585165 반응식
[CH2:1]([C:4]([CH2:13][C:14]#[CH:15])(C(OC)=O)[C:5]([O:7][CH3:8])=[O:6])[C:2]#[CH:3].[Cl-].[Na+]>CS(C)=O.O.COC(C)(C)C>[CH2:1]([CH:4]([CH2:13][C:14]#[CH:15])[C:5]([O:7][CH3:8])=[O:6])[C:2]#[CH:3]

참가 물질

6

반응물 2

HCID 5234Sodium ChlorideHCID 15468042,2-di-(prop-2-ynyl)-malonic acid dimethyl ester

생성물 1

HCID 12014811HCID 12014811, 화합물

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매2회HCID 15413tert-Butyl methyl ether용매

실험 절차

Dimethyl 2,2-di(2-propynyl)malonate (71 g) was treated to a Krapcho decarboxylation by heating at 170° C. with with sodium chloride (25 g) and water (23 ml) in dimethylsulfoxide (341 ml). After 15 hr, the solution was cooled and diluted with water and t-butyl methyl ether and extacted. The organic layer was washed with water (4×), brine, and then dried over sodium sulfate. Solvent removal afforded a liquid which was distilled, collecting the title compound at 109° C. (28 mm Hg).

후처리

  1. temperaturethe solution was cooled
  2. washThe organic layer was washed with water (4×), brine
  3. dry with materialdried over sodium sulfate
  4. customSolvent removal
  5. customafforded a liquid which
  6. distillationwas distilled
  7. customcollecting the title compound at 109° C. (28 mm Hg)

출처 및 근거

ORD 기록
ord-756f481218f849eb804b512e03a2efa7
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05936000

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