Cyanogen Bromide → HCID 87298019, 화합물

HRID 877854노트

반응식

HRID 877854 반응식
[CH2:1]([NH:3][C:4]1[C:9]([CH3:10])=[CH:8][CH:7]=[CH:6][C:5]=1[CH3:11])[CH3:2].[N:12]#[C:13]Br>C1(C)C=CC=CC=1>[CH2:1]([N:3]([C:13]#[N:12])[C:4]1[C:9]([CH3:10])=[CH:8][CH:7]=[CH:6][C:5]=1[CH3:11])[CH3:2]

참가 물질

4

반응물 2

HCID 10476Cyanogen BromideHCID 12539332N-Ethyl-2,6-dimethylaniline

생성물 1

HCID 87298019HCID 87298019, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

N-ethyl-2,6-dimethylaniline (5.9 g, 39.6 mmol) was added to a stirred solution of cyanogen bromide (2.1 g, 19.8 mmol) in toluene (50 mL). The reaction mixture was allowed to react overnight at room temperature during which a solid formed. A small temperature rise to 30° C. was observed. The suspension was filtered and the residue was washed with toluene (3×25 mL). The combined filtrates were evaporated to dryness by rotatory evaporation and the resulting residue was purified by Kugelrohr distillation (0.2 mbar, 110-125° C.) yielding a brown oil. Yield: 3.09 g (90%). The residue (N-ethyl-2,6-dimethylaniline hydrobromide) of the filtration step was used in the following synthetic step.

후처리

  1. customto react overnight at room temperature during which a solid
  2. customformed
  3. customto 30° C.
  4. filtrationThe suspension was filtered
  5. washthe residue was washed with toluene (3×25 mL)
  6. customThe combined filtrates were evaporated to dryness by rotatory evaporation
  7. distillationthe resulting residue was purified by Kugelrohr distillation (0.2 mbar, 110-125° C.)
  8. customyielding a brown oil
  9. filtrationThe residue (N-ethyl-2,6-dimethylaniline hydrobromide) of the filtration step

출처 및 근거

ORD 기록
ord-31b0cc3ef0124165a4394cea155ab67f
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987393B2

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