Lithium diisopropylamide → HCID 178505683、化合物

反応式

[Cl-].[Cl-].[CH:3]1([Ti+2:8][CH:9]2[CH:13]=[CH:12][CH:11]=[CH:10]2)[CH:7]=[CH:6][CH:5]=[CH:4]1.[F:14][C:15]1[CH:20]=[C:19]([F:21])[CH:18]=[CH:17][C:16]=1[CH2:22][CH2:23][CH2:24][N:25]1[CH:29]=[CH:28][CH:27]=[CH:26]1.[CH:30]([N-:33][CH:34]([CH3:36])C)([CH3:32])C.[Li+]>>[CH:9]1([Ti:8]([CH:3]2[CH:4]=[CH:5][CH:6]=[CH:7]2)([C:20]2[C:19]([F:21])=[CH:18][CH:17]=[C:16]([CH2:22][CH2:23][CH2:24][N:33]3[CH:30]=[CH:32][CH:36]=[CH:34]3)[C:15]=2[F:14])[C:20]2[C:19]([F:21])=[CH:18][CH:17]=[C:16]([CH2:22][CH2:23][CH2:24][N:25]3[CH:29]=[CH:28][CH:27]=[CH:26]3)[C:15]=2[F:14])[CH:13]=[CH:12][CH:11]=[CH:10]1

参加物

反応物 3

HCID 2724682Lithium diisopropylamide

HCID 199863711-[3-(2,4-Difluorophenyl)propyl]-1H-pyrrole

HCID 178420582HCID 178420582、化合物

生成物 1

HCID 178505683HCID 178505683、化合物収率 37.2%

実験手順

Analogously to Example 19, 2.5 g (0.010 mol) of bis(cyclopentadienyl)titanium dichloride and 4.9 g (0.022 mol) of 1-[3-(2,4-difluorophenyl)propyl]-1H-pyrrole are reacted with 0.022 mol of lithium diisopropylamide solution. The brown-orange oil is purified by means of flash chromatography using hexane/ethyl acetate (9:1) as solvent. 2.3 g of an orange glassy resin are obtained.

後処理

customThe brown-orange oil is purified by means of flash chromatography

出典と根拠

ORDレコード: ord-e13213effc694a24abf0a0b7c8c6edbb
出典データセット: uspto-grants-1991_11
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US05068371

反応ノート

読み込み中…