化工社
首页MCP工作台Skills
首页工作台通知我的
llms.txt · MCP 指南隐私政策 · 服务条款 · 支持v1.8.0
  1. 首页
  2. /反应

乙酸乙酯 → (R)-4-[(R)-1-(tert-Butoxy)ethyl]-3-(4-methoxybenzyl)oxazolidin-2-one

HRID 57504
笔记
打印预览

反应方程式

HRID 57504 反应方程式
C([O:8][C:9](=[O:21])[NH:10][C@@H:11]([C@H:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])[CH3:15])[CH2:12]O)C1C=CC=CC=1.[H-].[Na+].[CH3:24][O:25][C:26]1[CH:33]=[CH:32][C:29]([CH2:30]Cl)=[CH:28][CH:27]=1.CCOC(C)=O>CN(C=O)C.[I-].C([N+](CCCC)(CCCC)CCCC)CCC>[C:17]([O:16][C@@H:14]([C@H:11]1[CH2:12][O:21][C:9](=[O:8])[N:10]1[CH2:30][C:29]1[CH:32]=[CH:33][C:26]([O:25][CH3:24])=[CH:27][CH:28]=1)[CH3:15])([CH3:18])([CH3:19])[CH3:20]
参与物反应条件实验过程后处理来源与证据反应笔记

参与物

7

反应物 4

HCID 8857乙酸乙酯HCID 24758氢化钠HCID 699934-甲氧基氯苄HCID 59113072benzyl ((2R,3R)-3-(tert-butoxy)-1-hydroxybutan-2-yl)carbamate

产物 1

HCID 90422856(R)-4-[(R)-1-(tert-Butoxy)ethyl]-3-(4-methoxybenzyl)oxazolidin-2-one收率 96.5%

试剂、催化剂与溶剂 2

HCID 67553
四丁基碘化铵
催化剂
HCID 6228N,N-二甲基甲酰胺溶剂

反应条件

温度
0 °C

实验过程

To a solution of benzyl((2R,3R)-3-(tert-butoxy)-1-hydroxybutan-2-yl)carbamate (5.88 g, 19.9 mmol) in 100 mL DMF was added NaH (60% in mineral oil, 1.62 g, 40.6 mmol) at 0° C. The reaction mixture was stirred for 30 min at 0° C. To the reaction mixture were added 4-methoxybenzyl chloride (4.07 mL, 29.9 mmol) and tetrabutylammonium iodide (0.74 g, 1.99 mmol) and the resulting mixture was warmed to room temperature and stirred for 15.5 h. The reaction mixture was poured into ice water (200 mL) forming a white suspension. EtOAc (100 mL) was added and the resulting mixture was stirred for 5 min to form a clear two layer solution. After separation, the aqueous phase was extracted with EtOAc (100 mL×3). The combined organic solution was washed with brine (80 mL), dried over Na2SO4, filtered and concentrated. Flash column chromatography (EtOAc/Heptane 0 to 70%) gave 5.90 g of (R)-4-((R)-1-(tert-butoxy)ethyl)-3-(4-methoxybenzyl)oxazolidin-2-one with minor impurities. Major product 1H NMR (400 MHz, MeOD) δ 7.38-7.29 (m, 2H), 6.99-6.93 (m, 2H), 4.68-4.58 (m, 1H), 4.33 (dd, J=9.3, 4.5 Hz, 1H), 4.27-4.17 (m, 2H), 3.89 (dd, J=6.4, 4.8 Hz, 1H), 3.81 (s, 3H), 3.65 (dd, J=9.0, 4.6 Hz, 1H), 1.09 (s, 9H), 1.02 (d, J=6.3 Hz, 3H). MS m/z 308.2 (M+H).

后处理

  1. temperaturethe resulting mixture was warmed to room temperature
  2. stirringstirred for 15.5 h
  3. customforming a white suspension
  4. stirringthe resulting mixture was stirred for 5 min
  5. customto form a clear two layer solution
  6. customAfter separation
  7. extractionthe aqueous phase was extracted with EtOAc (100 mL×3)
  8. washThe combined organic solution was washed with brine (80 mL)
  9. dry with materialdried over Na2SO4
  10. filtrationfiltered
  11. concentrationconcentrated

来源与证据

ORD记录
ord-eeb454d1dc75494693aa19eccfa8f2f4
来源数据集
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
专利号
US09434719B2

反应笔记

加载中…

本页导航参与物反应条件实验过程后处理来源与证据反应笔记