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

Tetrahydrofuran → HCID 11689561、化合物

HRID 506275
ノート
印刷プレビュー

反応式

HRID 506275 の反応式
[C:1]([Mg]Br)#[C:2][CH3:3].C1COCC1.[N:11]12[CH2:18][CH2:17][CH:14]([CH2:15][CH2:16]1)[CH:13]([NH:19][C:20]([C:22]1[CH:23]=[CH:24][CH:25]=[C:26]3[O:30][C:29]([C:31]4[CH:36]=[CH:35][C:34](I)=[CH:33][CH:32]=4)=[N:28][C:27]=13)=[O:21])[CH2:12]2>CN(C=O)C.[Cl-].[Zn+2].[Cl-].Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[N:11]12[CH2:18][CH2:17][CH:14]([CH2:15][CH2:16]1)[CH:13]([NH:19][C:20]([C:22]1[CH:23]=[CH:24][CH:25]=[C:26]3[O:30][C:29]([C:31]4[CH:36]=[CH:35][C:34]([C:1]#[C:2][CH3:3])=[CH:33][CH:32]=4)=[N:28][C:27]=13)=[O:21])[CH2:12]2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 8028TetrahydrofuranHCID 11518485HCID 11518485、化合物HCID 178419101HCID 178419101、化合物

生成物 1

HCID 11689561HCID 11689561、化合物収率 88%

試薬・触媒・溶媒 3

HCID 3007855Zincchloride触媒HCID 178418476HCID 178418476、化合物
触媒
HCID 6228Dimethylformamide溶媒

実験手順

Zinc chloride (1.0 M in ether, 0.33 mL, 0.33 mmol) was added dropwise to a solution of 1-propynylmagnesium bromide in THF (0.5 M in THF, 0.66 mL, 0.33 mmol) at room temperature and the mixture was stirred under nitrogen for 10 min. N-(1-Azabicyclo[2.2.2]oct-3-yl)-2-(4-iodophenyl)benzoxazole-4-carboxamide (50 mg, 0.11 mmol) in DMF (2 mL) was added followed by bis(triphenylphosphine)dichloropalladium(II) (7.7 mg, 0.011 mmol). The resulting mixture was stirred under nitrogen at room temperature for 2 h, and then was quenched with saturated ammonium chloride, extracted with methylene chloride. The combined organic layers were washed with water and brine, dried (Na2SO4), filtered and concentrated. The crude material was purified by column chromatography (silica gel, 90:10:1 ethyl acetate/methanol/concentrated ammonium hydroxide) to afford N-(1-azabicyclo[2.2.2]oct-3-yl)-2-(4-propyn-1-ylphenyl)benzoxazole-4-carboxamide (36 mg, 88%) as a light yellow solid: 1H NMR (300 MHz, CDCl3) δ 9.56 (d, J=7.0 Hz, 1H), 8.23 (dd, J=8.0, 1.0 Hz, 1H), 8.17 (d, J=8.4 Hz, 2H), 7.73 (dd, J=8.0, 1.0 Hz, 1H), 7.58 (d, J=8.4 Hz, 2H), 7.49 (t, J=8.0 Hz, 1H), 4.35-4.29 (m, 1H), 3.54 (ddd, J=14.0, 9.5, 2.0 Hz, 1H), 3.16-2.82 (m, 5H), 2.20-2.03 (m, 2H), 2.14 (s, 3H), 1.80-1.60 (m, 3H); MS (ESI+) m/z 386 (M+H); HPLC>99% (AUC), tR=13.24 min.

後処理

  1. stirringThe resulting mixture was stirred under nitrogen at room temperature for 2 h
  2. customwas quenched with saturated ammonium chloride
  3. extractionextracted with methylene chloride
  4. washThe combined organic layers were washed with water and brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude material was purified by column chromatography (silica gel, 90:10:1 ethyl acetate/methanol/concentrated ammonium hydroxide)

出典と根拠

ORDレコード
ord-bedb136e2357486986809233a2ff0ddc
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07781430B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート