1-(Difluoromethoxy)-4-iodobenzene → 2-(3-{[4-(Difluoromethoxy)phenyl]ethynyl}phenyl)-1,3-dioxolane

HRID 30550

反応式

HRID 30550 の反応式
[C:1]([C:3]1[CH:4]=[C:5]([CH:9]2[O:13][CH2:12][CH2:11][O:10]2)[CH:6]=[CH:7][CH:8]=1)#[CH:2].[F:14][CH:15]([F:24])[O:16][C:17]1[CH:22]=[CH:21][C:20](I)=[CH:19][CH:18]=1>>[F:14][CH:15]([F:24])[O:16][C:17]1[CH:22]=[CH:21][C:20]([C:2]#[C:1][C:3]2[CH:4]=[C:5]([CH:9]3[O:10][CH2:11][CH2:12][O:13]3)[CH:6]=[CH:7][CH:8]=2)=[CH:19][CH:18]=1

参加物

3

反応物 2

HCID 27370081-(Difluoromethoxy)-4-iodobenzeneHCID 198973932-(3-Ethynylphenyl)-1,3-dioxolane

生成物 1

HCID 597903012-(3-{[4-(Difluoromethoxy)phenyl]ethynyl}phenyl)-1,3-dioxolane収率 85%

実験手順

Using essentially the same procedure described in Example 1, step a, and employing 2-(3-ethynylphenyl)-1,3-dioxolane and 1-(difluoromethoxy)-4-iodobenzene, the coupled product was obtained. This product was purified on silica gel (ISCO) using hexanes/EtOAc 5/1 as the eluting solvents to give 2-(3-{[4-(difluoromethoxy)phenyl]ethynyl}phenyl)-1,3-dioxolane as a yellow oil (7.9 g, 85% yield), MS m/e (M+H)+ 317; 1H NMR (400 MHz, DMSO-d6) 3.9-4.05 (m, 4H), 5.72 (s, 1H), 7.1-7.3 (m, 3H), 7.4 (m, 2H), 7.5-7.6 (m, 4H).

後処理

  1. customthe coupled product was obtained
  2. customThis product was purified on silica gel (ISCO)

出典と根拠

ORDレコード
ord-3e34a53d7190421e825142c2a2c4bcd8
出典データセット
uspto-grants-2008_09
特許番号
US07423158B2

関連ノート

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