Dimethylformamide dimethyl acetal → HCID 10975874, 화합물

HRID 1478238노트

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HRID 1478238 반응식
[CH2:1]([O:3][C:4](=[O:8])[CH2:5][N+:6]#[C-:7])[CH3:2].CO[CH:11](OC)[N:12]([CH3:14])[CH3:13]>C(O)C>[CH2:1]([O:3][C:4](=[O:8])/[C:5](/[N+:6]#[C-:7])=[CH:11]/[N:12]([CH3:14])[CH3:13])[CH3:2]

참가 물질

4

반응물 2

HCID 78373Dimethylformamide dimethyl acetalHCID 533707Ethyl isocyanoacetate

생성물 1

HCID 10975874HCID 10975874, 화합물수율 71.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of ethyl-2-isocyanoacetate (10.3 g, 91 mmol) in ethanol (100 ml) was cooled down to 0° C. 1,1-dimethoxy-N,N-dimethyl methanamine (26.6 ml, 200 mmol) was added and the reaction mixture was then allowed to reach RT and stirred for 24 h. The mixture was concentrated and the crude material was purified by flash chromatography (heptane/EtOAc, 100:0 to 40:60) to afford 11 g (64.7 mmol, 71.1% yield) of the title compound. LCMS: (M+H)=169; tR=0.74 min (LC-MS 2); 1H-NMR (CDCl3, 400 MHz) δ (ppm) 7.15 (s, 1H), 4.18 (q, 2H), 3.20 (bs, 6H), 1.26 (t, 3H).

후처리

  1. customto reach RT
  2. concentrationThe mixture was concentrated
  3. customthe crude material was purified by flash chromatography (heptane/EtOAc, 100:0 to 40:60)

출처 및 근거

ORD 기록
ord-07c576ca91d9475181cce6374cdb3277
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403827B2

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