Adamantane → Decyl adamantane

HRID 1609407

반응식

HRID 1609407 반응식
[CH2:1]=[CH:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[CH:11]12[CH2:20][CH:15]3[CH2:16][CH:17]([CH2:19][CH:13]([CH2:14]3)[CH2:12]1)[CH2:18]2.[Al](Br)(Br)Br>CCCCCC.C(Br)Br.[Al](Br)(Br)Br>[CH2:1]([C:11]12[CH2:20][CH:15]3[CH2:16][CH:17]([CH2:19][CH:13]([CH2:14]3)[CH2:12]1)[CH2:18]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]

참가 물질

7

반응물 3

HCID 9238AdamantaneHCID 133811-DeceneHCID 24409Aluminum bromide

생성물 1

HCID 22416186Decyl adamantane

시약·촉매·용매 3

HCID 24409Aluminum bromide촉매HCID 3024Dibromomethane용매HCID 8058Hexane용매

실험 절차

Decyl adamantane was prepared by reacting 140 g 1-decene, 54.4 gram adamantane in 100 cc n-hexane solvent and using 3 mmoles 1.0M AlBr3 in CH2Br2 or AlBr3 catalyst at 15°-50° C. reaction temperature. The product was isolated by quench the catalyst with dilute acid and aqueous work-up followed by distillation at 155° C. and 0.2 mm-Hg using a Kugelrohr to remove any C20 -material. The C30 + fraction was obtained in 80% yeild. It was hydrogenated at 200° C. and 500 psi H2 using 1 wt. % Ni/SiO2 catalyst.

후처리

  1. customat 15°-50° C.
  2. customreaction temperature
  3. customThe product was isolated
  4. customby quench the catalyst
  5. additionwith dilute acid and aqueous work-up
  6. distillationfollowed by distillation at 155° C.
  7. customto remove any C20 -material
  8. customThe C30 + fraction was obtained in 80% yeild
  9. customwas hydrogenated at 200° C.

출처 및 근거

ORD 기록
ord-d49e72834c184b4ca802e6b211731842
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05400427

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