Methylamine → 2,4-Dibromo-N-methylbutanamide

温度

30 °C

2,4-Dibromobutanoyl chloride (CAS no. 82820-87-9) (16.9 g, 64 mmol) in DCM (20 mL) was added dropwise to a solution of methylamine (20 mL) in water (30 mL) and DCM (30 mL) at 10-15° C., then warmed to 30° C. and stirred for 30 minutes. The organic layer was separated and the aqueous layer re-extracted with DCM (2×10 mL), the combined organic layers were washed with brine (20 mL), dried (MgSO4) and evaporated to afford the product (16.3 g, 98%). 1H NMR δ (400 MHz, CDCl3) 2.35-2.45 (m, 1H), 2.57-2.67 (m, 1H), 2.81 (d, 3H), 3.44-3.54 (m, 2H), 4.46 (q, 1H), 6.34 (s, 1H).

1. customThe organic layer was separated
2. extractionthe aqueous layer re-extracted with DCM (2×10 mL)
3. washthe combined organic layers were washed with brine (20 mL)
4. dry with materialdried (MgSO4)
5. customevaporated

ORDレコード

ord-506f290a0dd440b7a851b96b62e8f482

出典データセット

uspto-grants-2011_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07902200B2