Carbon tetrabromide → HCID 20076910、化合物

HRID 1654769ノート

反応式

HRID 1654769 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 20076910HCID 20076910、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-91889ad73b3844179e2a58ea06048878
出典データセット
uspto-grants-1995_04
特許番号
US05409942

反応ノート

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