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 → 1-Oxo-1-[5-(2-pyridyl)oxazol-2-yl]-3-(4-(benzyloxy)phenyl)propane

HRID 386426
ノート
印刷プレビュー

反応式

HRID 386426 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1[O:11][CH:10]=[N:9][CH:8]=1.[Li][CH2:13][CH2:14][CH2:15][CH3:16].[OH:17][C:18]1[CH:23]=[CH:22][C:21]([CH2:24][CH2:25][C:26](Cl)=[O:27])=[CH:20][CH:19]=1.[CH2:29]1[CH2:33]OC[CH2:30]1>[Cl-].[Cl-].[Zn+2].[Cu]I>[O:27]=[C:26]([C:10]1[O:11][C:7]([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=2)=[CH:8][N:9]=1)[CH2:25][CH2:24][C:21]1[CH:22]=[CH:23][C:18]([O:17][CH2:16][C:15]2[CH:33]=[CH:29][CH:30]=[CH:13][CH:14]=2)=[CH:19][CH:20]=1
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

7

反応物 4

HCID 8028Tetrahydrofuran3 回HCID 7371945-(2-Pyridyl)oxazoleHCID 866458123-(4-Hydroxyphenyl)propanoyl chlorideHCID 178418339Butyllithium

生成物 1

HCID 167351591-Oxo-1-[5-(2-pyridyl)oxazol-2-yl]-3-(4-(benzyloxy)phenyl)propane収率 33%

試薬・触媒・溶媒 2

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
触媒
HCID 3007855Zincchloride触媒

反応条件

温度
-78 °C

実験手順

A solution of 5-(2-pyridyl)oxazole (Saikachi, H., et al. Chem. Pharm. Bull. 1969, 27, 793-796; 116 mg, 0.794 mmol) in anhydrous THF (4 mL) at −78° C. was treated dropwise with a solution of n-BuLi in hexanes (1.6 M, 0.64 mL, 0.953 mmol) under N2 and the resulting solution was stirred at −78° C. for 35 min. A solution of ZnCl2 in THF (0.5 M, 1.9 mL, 1.56 mmol) was added and the mixture was allowed to warm to 0° C. After stirring at 0° C. for 45 min, CuI (160 mg, 0.840 mmol) was added. After the mixture was stirred at 0° C. for 15 min, a solution of 3-(4-hydroxyphenyl)propanoyl chloride (1.2 equiv; prepared from 3-(4-(benzyloxy)phenyl)propanoic acid and oxalyl chloride) in anhydrous THF (1.5 mL) was added dropwise, and the mixture was stirred for an additional 1 h. The reaction mixture was quenched with addition of saturated aqueous NaHCO3 and extracted with EtOAc. The organic layer was filtered through diatomaceous earth, dried over anhydrous Na2SO4, filtered and evaporated to yield the crude product. Column chromatography (SiO2, 2.5×5 cm, 10-30% EtOAc-hexanes gradient) followed by PTLC (SiO2, 50% EtOAc-hexanes) afforded the title compound (33%) as a white solid: mp 99-100° C. 1H NMR (CDCl3, 400 MHz) 8.67 (app d, J=4.4 Hz, 1H), 7.88 (s, 1H), 7.87-7.85 (m, 1H), 7.81 (td, 1H, J=7.8, 1.8 Hz), 7.44 (d, 2H, J=7.0 Hz), 7.39 (t, 2H, J=7.5 Hz), 7.32 (t, 2H, J=6.8 Hz), 7.19 (d, 2H, J=8.5 Hz), 6.91 (d, 2H, J=8.5 Hz), 5.04 (s, 2H), 3.44 (t, 2H, J=7.4 Hz), 3.06 (t, 2H, J=7.4 Hz); 13C NMR (CDCl3, 100 MHz) 187.4, 157.2 (2C), 153.2, 150.1, 146.2, 137.1, 137.0, 132.7, 129.4, 128.5, 127.9, 127.4, 126.9, 124.2, 120.4, 114.9, 70.0, 40.9, 28.9; IR (film) νmax 3097, 2919, 1693, 1602, 1582, 1514, 1470, 1427, 1382, 1253, 1177, 1042, 963, 938, 785, 741, 697 cm−1; ESI-TOF m/z 385.1549 (C24H20N2O3+H+ requires 385.1547).

後処理

  1. temperatureto warm to 0° C
  2. stirringAfter stirring at 0° C. for 45 min
  3. stirringAfter the mixture was stirred at 0° C. for 15 min
  4. stirringthe mixture was stirred for an additional 1 h
  5. customThe reaction mixture was quenched with addition of saturated aqueous NaHCO3
  6. extractionextracted with EtOAc
  7. filtrationThe organic layer was filtered through diatomaceous earth
  8. dry with materialdried over anhydrous Na2SO4
  9. filtrationfiltered
  10. customevaporated
  11. customto yield the crude product

出典と根拠

ORDレコード
ord-111584b818534f139be34013495a78c0
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08372823B2

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