甲胺-D5 → N-甲基-1,4-二噁螺[4.5]-8-癸胺 (弗洛中间体)

HRID 1663018笔记

反应方程式

HRID 1663018 反应方程式
[O:1]1[C:5]2([CH2:10][CH2:9][C:8](=O)[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.C(Cl)Cl.CN.[C:17]([BH3-])#[N:18].[Na+]>C(O)(=O)C>[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([NH:18][CH3:17])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1

参与物

6

反应物 4

HCID 6329甲胺-D5HCID 6344二氯甲烷HCID 5674151,4-环己二酮单乙二醇缩酮HCID 5003444氰基硼氢化钠

产物 1

HCID 16786570N-甲基-1,4-二噁螺[4.5]-8-癸胺 (弗洛中间体)收率 43.8%

试剂、催化剂与溶剂 1

HCID 176醋酸溶剂

实验过程

A solution of 1,4-dioxa-spiro[4.5]decan-8-one (3.1 g, 20 mmol) and CH2Cl2 (50 mL) was stirred with methylamine (15 mL, 30 mmol, 2.0M solution in THF), sodium cyanoborohydride (1.3 g, 20 mmol), and acetic acid (0.1 mL) at room temperature. After 8 hours, the reaction mixture was washed with water (50 mL) and concentrated. The residue was purified by flash chromatography to afford 1.5 g of (1,4-dioxa-spiro[4.5]dec-8-yl)-methyl-amine as an oil.

后处理

  1. washthe reaction mixture was washed with water (50 mL)
  2. concentrationconcentrated
  3. customThe residue was purified by flash chromatography

来源与证据

ORD记录
ord-4554f1545a354faca8a7824f54180310
来源数据集
uspto-grants-2011_10
专利号
US08034826B2

反应笔记

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