2-Isopropylphenol → HCID 54321892、化合物

HRID 275232

反応式

HRID 275232 の反応式
[H-].[Na+].[CH:3]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[OH:12])([CH3:5])[CH3:4].[P:13]([Cl:17])(Cl)(Cl)=[S:14]>C1(C)C=CC=CC=1>[P:13]([Cl:17])([O:12][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[CH:3]([CH3:5])[CH3:4])([O:12][C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=1[CH:3]([CH3:5])[CH3:4])=[S:14]

参加物

5

反応物 3

HCID 69432-IsopropylphenolHCID 19883Thiophosphoryl chlorideHCID 24758Sodium hydride

生成物 1

HCID 54321892HCID 54321892、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Sodium hydride (38.0 g of 80% suspension in mineral oil) was added to a stirred solution of 2-isopropylphenol (139.2 g) and thiophosphoryl chloride (84.5 g) in toluene (500 cm3) at such a rate that the reaction temperature did not rise above 65° C. After stirring for a further 0.5 hr at ambient temperature, the solution was extracted twice with water (250 cm3 portions), separated, dried (MgSO4) and concentrated by distillation of solvents under reduced pressure yielding crude bis(2-isopropylphenyl) chlorothiophosphate, a brown oil (164.2 g); 31P NMR in CDCl3, singlet 53.0 ppm downfield of H3PO4). Of this material, 54.0 g were reacted with ammonia by the procedure of Example 9 yielding crude bis(2-isopropylphenyl)thiophosphoramide) (50.0 g; 31PNmr, singlet δ=58.8 ppm).

後処理

  1. customdid not rise above 65° C
  2. extractionthe solution was extracted twice with water (250 cm3 portions)
  3. customseparated
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated by distillation of solvents under reduced pressure

出典と根拠

ORDレコード
ord-9bda1c41ff1141698c0a778d0d368348
出典データセット
uspto-grants-1995_02
特許番号
US05393431

関連ノート

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