Ethyl Heptanoate → Dimethyl (2-oxooctyl)phosphonate

HRID 66242노트

반응식

HRID 66242 반응식
[CH3:1][P:2](=[O:7])([O:5][CH3:6])[O:3][CH3:4].O1CCCC1.[C:13](OCC)(=[O:20])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]>C(O)(=O)C>[O:20]=[C:13]([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])[CH2:1][P:2](=[O:7])([O:5][CH3:6])[O:3][CH3:4]

참가 물질

5

반응물 3

HCID 7797Ethyl HeptanoateHCID 8028Tetrahydrofuran2회HCID 12958Dimethyl methylphosphonate

생성물 1

HCID 13390134Dimethyl (2-oxooctyl)phosphonate

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

n-Butyllithiium (130 ml. of 1.6 M. solution) is slowly added to a solution of dimethyl methylphosphonate (25.6 g.) in 475 ml. of tetrahydrofuran (THF) at about -65° C. To the mixture is added a solution of ethyl heptanoate (18.4 g.) in 50 ml. of THF, annd the resulting mixture is stirred at about -70° C. for 2 hrs. Then, 16 ml. of acetic acid is added, and the mixture is concentrated under reduced pressure. The residue is mixed with dichloromethane (about 400 ml.) and water (about 50 ml.) shaken, and separated. The organic phase is dried over magnesium sulfate and concentrated. Distillation yields the title compound.

후처리

  1. customat about -65° C
  2. concentrationthe mixture is concentrated under reduced pressure
  3. additionThe residue is mixed with dichloromethane (about 400 ml.) and water (about 50 ml.)
  4. customseparated
  5. dry with materialThe organic phase is dried over magnesium sulfate
  6. concentrationconcentrated
  7. distillationDistillation

출처 및 근거

ORD 기록
ord-c2faf03a3fe7473386599f958ca774fd
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04130721

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