Acetic Acid → 3-Methyl-2-oxooct-6-inylphosphonic acid dimethyl ester

HRID 905255

반응식

HRID 905255 반응식
[CH2:1]([Li])CCC.[CH3:6][P:7]([OH:10])(=O)[OH:8].C(O[C:14](=[O:22])[CH:15]([CH3:21])[CH2:16][CH2:17][C:18]#[C:19][CH3:20])C.[C:23]([OH:26])(=O)C>CCCCCC.O1CCCC1>[CH3:1][O:8][P:7]([CH2:6][C:14](=[O:22])[CH:15]([CH3:21])[CH2:16][CH2:17][C:18]#[C:19][CH3:20])(=[O:10])[O:26][CH3:23]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 13818Methylphosphonic acidHCID 536913892-Methylhept-5-ynoic acid ethyl esterHCID 178418339Butyllithium

생성물 1

HCID 538600643-Methyl-2-oxooct-6-inylphosphonic acid dimethyl ester

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8058Hexane용매

실험 절차

At -70° C., 73 ml of a 1.7-molar butyllithium solution in hexane is added dropwise to a solution of 18.6 g of the dimethyl ester of methanephosphonic acid in 280 ml of tetrahydrofuran; the mixture is stirred for 15 minutes and a solution of 10.5 g of 2-methylhept-5-ynoic acid ethyl ester in 48 ml of tetrahydrofuran is gradually added thereto. The mixture is stirred for 4 hours at -70° C., neutralized with acetic acid, and evaporated under vacuum. The distillation of the residue under vacuum at 0.6 torr and 130° C. yields 10.8 g of the title compound as a colorless fluid.

후처리

  1. stirringThe mixture is stirred for 4 hours at -70° C.
  2. customevaporated under vacuum
  3. distillationThe distillation of the residue under vacuum at 0.6 torr and 130° C.

출처 및 근거

ORD 기록
ord-1f1123aa3c8649288837c9d8507ab92f
출처 데이터셋
uspto-grants-1983_12
특허 번호
US04423067

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