ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Water → (2,6-Diisopropylphenyl)[1-(2'-methoxybiphenyl-3-yl)ethylidene]amine

HRID 45478
ノート
印刷プレビュー

反応式

HRID 45478 の反応式
Br[C:2]1[CH:3]=[C:4]([C:8](=[N:10][C:11]2[C:16]([CH:17]([CH3:19])[CH3:18])=[CH:15][CH:14]=[CH:13][C:12]=2[CH:20]([CH3:22])[CH3:21])[CH3:9])[CH:5]=[CH:6][CH:7]=1.[Li]CCCC.Br[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=1[O:35][CH3:36].O>C1COCC1.[Cl-].[Cl-].[Zn+2].CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C>[CH:20]([C:12]1[CH:13]=[CH:14][CH:15]=[C:16]([CH:17]([CH3:19])[CH3:18])[C:11]=1[N:10]=[C:8]([C:4]1[CH:3]=[C:2]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=2[O:35][CH3:36])[CH:7]=[CH:6][CH:5]=1)[CH3:9])([CH3:22])[CH3:21]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 962WaterHCID 113582-BromoanisoleHCID 58238584N-[1-(3-Bromophenyl)ethylidene]-2,6-diisopropylanilineHCID 178418339Butyllithium

生成物 1

HCID 58238573(2,6-Diisopropylphenyl)[1-(2'-methoxybiphenyl-3-yl)ethylidene]amine収率 79%

試薬・触媒・溶媒 3

HCID 3007855
Zincchloride
触媒
HCID 178418851HCID 178418851、化合物触媒
HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-70 °C

実験手順

To a solution of 2.78 g (7.75 mmol) of 13 in 30 mL of THF, 3.10 mL (7.75 mmol) of 2.5 M nBuLi in hexanes was added at −100° C. The reaction mixture was stirred for 1 hr at −70° C., then cooled to −100° C., and 8.35 mL (8.35 mmol) of 1M ZnCl2 in THF was added. The resulting mixture was slowly warmed to room temperature, stirred for 12 hr at this temperature, and then 1.45 g (7.75 mmol) of 2-bromoanisole and 85 mg (0.15 mmol) of Pd(PtBu3)2 were added. The resulting mixture was refluxed for 3 hr, and then 5 mL of water was added. This mixture was passed through short layer of silica gel 60 (40-63 um) which was then additionally washed with 30 mL of dichloromethane. The combined organic filtrate was evaporated to dryness, and the product was isolated by flash chromatography on silica gel 60(40-63 um, eluent: from hexanes to hexanes-diethyl ether=20:1, vol.). This procedure gave 2.36 g (79%) of the title product.

後処理

  1. temperaturecooled to −100° C.
  2. temperatureThe resulting mixture was slowly warmed to room temperature
  3. stirringstirred for 12 hr at this temperature
  4. temperatureThe resulting mixture was refluxed for 3 hr
  5. washwas then additionally washed with 30 mL of dichloromethane
  6. customThe combined organic filtrate was evaporated to dryness
  7. customthe product was isolated by flash chromatography on silica gel 60(40-63 um, eluent: from hexanes to hexanes-diethyl ether=20:1, vol.)

出典と根拠

ORDレコード
ord-48ce2117ca204564bb083007c42e29cc
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08541522B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート