Hydrochloric Acid → Methyl 4-[2-(imidazol-2-yl)ethyl]benzoate hydrochloride

HRID 583686ノート

反応式

HRID 583686 の反応式
[C:1]([CH2:3][CH2:4][C:5]1[CH:14]=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[CH:7][CH:6]=1)#[N:2].CO.[ClH:17].CO[CH:20](OC)[CH2:21][NH2:22]>CCOCC>[ClH:17].[NH:2]1[CH:20]=[CH:21][N:22]=[C:1]1[CH2:3][CH2:4][C:5]1[CH:14]=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[CH:7][CH:6]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 89728Aminoacetaldehyde dimethyl acetalHCID 13308299Methyl 4-(2-cyanoethyl)benzoate

生成物 1

HCID 18928585Methyl 4-[2-(imidazol-2-yl)ethyl]benzoate hydrochloride

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Nitrile 23-3 (400 mg, 2.11 mmol) was dissolved in 10 mL Et2O at 0° MeOH (289 μL, 4.2 mmol) was added, the mixture was saturated with anhydrous HCl. Once the white ppt. formed, the solvent was evaporated and replaced with MeOH (5 mL), cooled to 0°, and aminoacetaldehyde dimethylacetal (250 μL, 2.3 mmol) was added. The reaction was heated to reflux for 3 days then concentrated, diluted in 10 mL 6N HCl and concentrated again providing 23-4 as a solid.

後処理

  1. additionwas added
  2. customformed
  3. customthe solvent was evaporated
  4. temperaturecooled to 0°
  5. temperatureThe reaction was heated
  6. temperatureto reflux for 3 days
  7. concentrationthen concentrated
  8. additiondiluted in 10 mL 6N HCl
  9. concentrationconcentrated again

出典と根拠

ORDレコード
ord-d853fbbf2d42476e87b82191a538b8ab
出典データセット
uspto-grants-1999_07
特許番号
US05929120

反応ノート

読み込み中…