Methylamine → N-methyl-1,4-dioxaspiro(4.5)decan-8-amine

HRID 1663018노트

반응식

HRID 1663018 반응식
[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

참가 물질

6

반응물 4

HCID 6329MethylamineHCID 6344DichloromethaneHCID 5674151,4-Dioxaspiro[4.5]decan-8-oneHCID 5003444Sodium cyanoborohydride

생성물 1

HCID 16786570N-methyl-1,4-dioxaspiro(4.5)decan-8-amine수율 43.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-4554f1545a354faca8a7824f54180310
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08034826B2

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