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N,N-二异丙基乙胺 → (S)-4-Methyl-2-[methyl-(3-methyl-but-2-enyl)-amino]-pentanoic acid

HRID 1069447
笔记
打印预览

反应方程式

HRID 1069447 反应方程式
[CH3:1][N:2]([C:11](OC(C)(C)C)=O)[C@H:3]([C:8]([OH:10])=[O:9])[CH2:4][CH:5]([CH3:7])[CH3:6].CN(C(ON1N=NC2C=C[CH:31]=[CH:32][C:27]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH:42](N(C(C)C)CC)(C)C>CC#N>[CH3:7][CH:5]([CH3:6])[CH2:4][C@H:3]([N:2]([CH3:1])[CH2:11][CH:42]=[C:32]([CH3:31])[CH3:27])[C:8]([OH:10])=[O:9]
参与物实验过程后处理来源与证据反应笔记

参与物

5

反应物 3

HCID 81531N,N-二异丙基乙胺HCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 7010555N-叔丁氧羰基-N-甲基-L-亮氨酸

产物 1

HCID 86757058(S)-4-Methyl-2-[methyl-(3-methyl-but-2-enyl)-amino]-pentanoic acid收率 340.9%

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂
本页导航参与物实验过程后处理来源与证据反应笔记

实验过程

A mixture of Ia (0.535 g, 1.65 mmol), N-Methyl-N-Boc-L-Leucine (0.405 g, 1.65 mmol), HBTU (0.625 g, 1.65 mmol), and diisopropylethylamine (0.516 g, 6.6 mmol) was stirred in CH3CN (30 mL) for 15 hours. The reaction mixture was concentrated, redissolved in EtOAc, washed 3 times with saturated sodium bicarbonate solution and once with brine, then concentrated to give 1.2 g of the desired product.

后处理

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionredissolved in EtOAc
  3. washwashed 3 times with saturated sodium bicarbonate solution
  4. concentrationonce with brine, then concentrated

来源与证据

ORD记录
ord-c752f89a232f4a87b821ba16bcddcadc
来源数据集
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
专利号
US06251918B1

反应笔记

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