N-乙酰-L-亮氨酸 → (1S)-5-tert-butyl-2,3-dihydro-1H-inden-1-amine

HRID 451598

反应方程式

HRID 451598 反应方程式
[C:1]([C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[CH:10]([NH2:14])[CH2:9][CH2:8]2)([CH3:4])([CH3:3])[CH3:2].C(N[C@H](C(O)=O)CC(C)C)(=O)C>CO>[C:1]([C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][CH:13]=1)[C@@H:10]([NH2:14])[CH2:9][CH2:8]2)([CH3:4])([CH3:2])[CH3:3]

参与物

4

反应物 2

HCID 70912N-乙酰-L-亮氨酸HCID 115066015-叔丁基-2,3-二氢-1H-茚-1-胺

产物 1

HCID 24777891(1S)-5-tert-butyl-2,3-dihydro-1H-inden-1-amine

试剂、催化剂与溶剂 1

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂

反应条件

温度
65 °C

实验过程

5-tert-Butyl-2,3-dihydro-1H-inden-1-ylamine (25.51 g, 93% potency), N-acetyl-(L)-leucine (23.34 g), and methanol (315 mL) were combined and heated at 65° C. for 1 hour. The solution was allowed to cool to ambient temperature. The solids were filtered and washed with toluene. The solid was then resuspended in methanol (125 mL) and brought to reflux. The solution was allowed to cool to ambient temperature and the solids were filtered. The solid was dried at 40° C. under reduced pressure to provide the title compound (98.7% ee).

后处理

  1. temperatureto cool to ambient temperature
  2. filtrationThe solids were filtered
  3. washwashed with toluene
  4. temperatureto reflux
  5. temperatureto cool to ambient temperature
  6. filtrationthe solids were filtered
  7. customThe solid was dried at 40° C. under reduced pressure

来源与证据

ORD记录
ord-cbdd40558afe41ffaa64d1cb2a577c28
来源数据集
uspto-grants-2013_07
专利号
US08487116B2

关联笔记

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