1-Bromooctadecane → n-Octadecyl Dicyclohexylphosphinodithioate

HRID 461608

반응식

HRID 461608 반응식
[CH:1]1([P:7]([CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)([SH:9])=[S:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:16](Br)[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH3:33]>CC(C)=O>[CH:1]1([P:7]([CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)([S:9][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][CH3:16])=[S:8])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

참가 물질

4

반응물 2

HCID 82181-BromooctadecaneHCID 75641Phosphinodithioic acid, dicyclohexyl-

생성물 1

HCID 21391648n-Octadecyl Dicyclohexylphosphinodithioate수율 77.8%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To 14.0 g. (0.05 m.) of the ammonium salt of dicyclohexylphosphinodithioic acid in 250 mls. of acetone was added 16.67 g. (0.05 m.) of n-octadecylbromide and the mixture was refluxed for 15 hours. The precipitate was then separated by filtration and the filtrate was cooled to precipitate a crystalline solid. The crystalline material was filtered off and recrystallized from acetone to obtain 20 g. (77.8% yield) of product which melted at 67°-69° C.

후처리

  1. customThe precipitate was then separated by filtration
  2. temperaturethe filtrate was cooled
  3. customto precipitate a crystalline solid
  4. filtrationThe crystalline material was filtered off
  5. customrecrystallized from acetone
  6. customto obtain 20 g

출처 및 근거

ORD 기록
ord-457ee94ea6cf49e78ef04328c9ee3c63
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04064106

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