1H-Indene, 2-(1-methylethyl)-4-phenyl- → Lithium 2-isopropyl-4-phenylindenide

HRID 1595108ノート

反応式

HRID 1595108 の反応式
[CH:1]([C:4]1[CH2:5][C:6]2[C:11]([CH:12]=1)=[C:10]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH:9]=[CH:8][CH:7]=2)([CH3:3])[CH3:2].C([Li:23])CCC>C1(C)C=CC=CC=1>[CH:1]([C:4]1[CH-:5][C:6]2[C:11]([CH:12]=1)=[C:10]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH:9]=[CH:8][CH:7]=2)([CH3:3])[CH3:2].[Li+:23]

参加物

4

反応物 2

HCID 180082381H-Indene, 2-(1-methylethyl)-4-phenyl-HCID 178418339Butyllithium

生成物 1

HCID 22023052Lithium 2-isopropyl-4-phenylindenide収率 93.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a toluene solution (25 ml) of 2-isopropyl-4-phenylindene (3.34 g, 14.25 mmol), in a glovebox filled with argon, was added n-butyl lithium (5.500 ml, 13.75 mmol). The mixture was stirred at room temperature overnight. The toluene was removed under reduced pressure. Hexane (20 ml) was added and removed under reduced pressure then added again (50 ml). The mixture was stirred for 1 h then filtered, washed with about 15 ml hexane and the filtrate dried under vacuum. The lithium indenide product (3.09 g) was obtained as an orange-brown powder. This material was stored in the glovebox until needed.

後処理

  1. customThe toluene was removed under reduced pressure
  2. additionHexane (20 ml) was added
  3. customremoved under reduced pressure
  4. additionthen added again (50 ml)
  5. stirringThe mixture was stirred for 1 h
  6. filtrationthen filtered
  7. washwashed with about 15 ml hexane
  8. customthe filtrate dried under vacuum

出典と根拠

ORDレコード
ord-0b5fdc7fdcb94c1e9053fdd10e30b0e2
出典データセット
uspto-grants-2001_09
特許番号
US06284905B1

反応ノート

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