Adamantane → Decyl adamantane

HRID 1721536

反応式

HRID 1721536 の反応式
[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]

参加物

7

反応物 3

HCID 9238AdamantaneHCID 133811-DeceneHCID 24409Aluminum bromide

生成物 1

HCID 22416186Decyl adamantane収率 80%

試薬・触媒・溶媒 3

HCID 24409Aluminum bromide触媒HCID 3024Dibromomethane溶媒HCID 8058Hexane溶媒

実験手順

Decyl adamantane was prepared by reacting 140 g 1-decene, 54.4 gram adamantane in 100 cc n-hexane solvent and using 3 mmoles 1.0 M 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% yield. It was hydrogenated at 200° C. and 500 psi H2 using 1 wt.% Ni/SiO2 catalyst.

後処理

  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% yield
  9. customwas hydrogenated at 200° C.

出典と根拠

ORDレコード
ord-eb5ed5f794d344f385376cf196d3d376
出典データセット
uspto-grants-1996_04
特許番号
US05510549

関連ノート

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