Thymol → Bis(2-isopropyl-5-methylphenyl) chlorothiophosphate

HRID 275234

反応式

HRID 275234 の反応式
[CH:1]([C:4]1[CH:9]=[CH:8][C:7]([CH3:10])=[CH:6][C:5]=1[OH:11])([CH3:3])[CH3:2].[H-].[Na+].[P:14]([Cl:18])(Cl)(Cl)=[S:15]>>[P:14]([Cl:18])([O:11][C:5]1[CH:6]=[C:7]([CH3:10])[CH:8]=[CH:9][C:4]=1[CH:1]([CH3:3])[CH3:2])([O:11][C:5]1[CH:6]=[C:7]([CH3:10])[CH:8]=[CH:9][C:4]=1[CH:1]([CH3:3])[CH3:2])=[S:15]

参加物

4

反応物 3

HCID 6989ThymolHCID 19883Thiophosphoryl chlorideHCID 24758Sodium hydride

生成物 1

HCID 19690221Bis(2-isopropyl-5-methylphenyl) chlorothiophosphate収率 63%

実験手順

2-isopropyl-5-methylphenol was reacted with sodium hydride and thiophosphoryl chloride using the procedure of Example 21 to form bis(2-isopropyl-5-methylphenyl) chlorothiophosphate (31PNMR, singlet, 57 ppm). This compound was reacted with diphenylphosphonothioic amide by the General Method C(ii) (THF) yielding the compound of Formula I in which R1 =R2 =phenyl and R3 =R4 =2-isopropyl-5-methylphenoxy. Yield 63%; titration purity, 90%, MW593; 31PNMR, quartet 53ppm. Test 2 (Table 2) showed that the product is a very strong extractant for zinc; however on long standing it crystallised from ESCAID® solution.

出典と根拠

ORDレコード
ord-1ade696d41b14a8697f345a89fba609b
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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