Potassium Hydroxide → HCID 13343963, 화합물

HRID 1461978

반응식

HRID 1461978 반응식
[S:1]([C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.[P:16](=[O:25])(Cl)([S:20][CH2:21][CH2:22][CH3:23])[O:17][CH2:18][CH3:19].[OH-:26].[K+].C1CC2OCCOCCOC3C(OCCO[CH2:51][CH2:52][O:53]C2CC1)CCCC3>C(#N)C>[CH2:18]([O:17][P:16]([O:8][C:5]1[CH:6]=[CH:7][C:2]([S:1][C:9]2[CH:14]=[CH:13][C:12]([O:15][P:16]([O:53][CH2:52][CH3:51])([S:20][CH2:21][CH2:22][CH3:23])=[O:26])=[CH:11][CH:10]=2)=[CH:3][CH:4]=1)([S:20][CH2:21][CH2:22][CH3:23])=[O:25])[CH3:19]

참가 물질

6

반응물 4

HCID 14797Potassium HydroxideHCID 175704,4'-ThiodiphenolHCID 85955Dicyclohexano-18-crown-6HCID 11745722O-Ethyl S-propyl chlorothiophosphate

생성물 1

HCID 13343963HCID 13343963, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a 250 ml round bottom flask was added 4,4'-thiodiphenol (4.36 g, 20 mmol), O-ethyl S-n-propyl phosphorochloridothioate (9.12 g, 45 mmol), powdered potassium hydroxide (3.37 g, 60 mmol), dicyclohexano-18-crown-6 (catalytic quantity), and acetonitrile. This mixture was refluxed 14 hours, cooled to room temperature, and the organic soluble fraction decanted from the solids. The organic solution was diluted with ether and successively washed with 4M NaOH (3×100 ml), water (2×50 ml), 5% HCl (1×50 ml), water (2×50 ml), and brine (2×50 ml). After drying (MgSO4) the solution was concentrated under reduced pressure to give a colorless oil (4.8 g, 7.6 mmol).

후처리

  1. temperatureThis mixture was refluxed 14 hours
  2. customthe organic soluble fraction decanted from the solids
  3. additionThe organic solution was diluted with ether
  4. washsuccessively washed with 4M NaOH (3×100 ml), water (2×50 ml), 5% HCl (1×50 ml), water (2×50 ml), and brine (2×50 ml)
  5. dry with materialAfter drying (MgSO4) the solution
  6. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-fc5b32dd410548f1b4fb89eab4fa1bc5
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04457922

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