Carbon tetrabromide → HCID 20076910, 화합물

HRID 1654769노트

반응식

HRID 1654769 반응식
[C:1]([Br:5])(Br)(Br)[Br:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[NH:25]1[CH:29]=[CH:28][N:27]=[C:26]1[CH:30]=O>C(Cl)Cl>[Br:2][C:1]([Br:5])=[CH:30][C:26]1[NH:25][CH:29]=[CH:28][N:27]=1

참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 249551H-imidazole-2-carbaldehyde

생성물 1

HCID 20076910HCID 20076910, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

반응 조건

온도
0 °C

실험 절차

Mix carbon tetrabromide (49.8 g, 150 mmol) and methylene chloride (75 mL) and cool to 0° C. Add, by dropwise addition, a solution of triphenylphosphine (78.6 g, 300 mmol) in methylene chloride (75 mL). Stir at 0° C. for 30 minutes. Add, by dropwise addition, a solution of 2-imidazolecarboxaldehyde (7.57 g, 78.8 mmol) in methylene chloride (75 mL). Remove the cooling bath and stir at room temperature until the reaction is complete. Pour onto ethyl ether and water, separate the organic layer and dry (MgO4). Filter and evaporate the solvent in vacuo. Purify by silica gel chromatography to yield the title compound.

후처리

  1. additionAdd, by dropwise addition
  2. additionAdd, by dropwise addition
  3. customRemove the cooling bath
  4. stirringstir at room temperature until the reaction
  5. additionPour onto ethyl ether and water
  6. customseparate the organic layer
  7. customdry (MgO4)
  8. filtrationFilter
  9. customevaporate the solvent in vacuo
  10. customPurify by silica gel chromatography

출처 및 근거

ORD 기록
ord-91889ad73b3844179e2a58ea06048878
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05409942

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