Potassium Hydroxide → HCID 13343963、化合物

HRID 1461978

反応式

HRID 1461978 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 13343963HCID 13343963、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fc5b32dd410548f1b4fb89eab4fa1bc5
出典データセット
uspto-grants-1984_07
特許番号
US04457922

関連ノート

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