Hydrochloric Acid → HCID 19876799、化合物

HRID 1886040ノート

反応式

HRID 1886040 の反応式
[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[N:4]=[C:3]1[NH:11][CH2:12][CH2:13][NH:14]C(=O)C.Cl>CO>[NH2:14][CH2:13][CH2:12][NH:11][C:3]1[N:2]([CH3:1])[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[N:4]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 19876826HCID 19876826、化合物

生成物 1

HCID 19876799HCID 19876799、化合物収率 77.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of N-[2-[(1-methyl-1H-benzimidazol-2-yl)amino]ethyl]acetamide (2.32 g, 9.98 mmol), 2N HCl (20 mL), and MeOH (20 mL) was heated under reflux for 20 hours. The mixture was concentrated, diluted with H2O, made basic (pH9) with 2.5N NaOH, and extracted with EtOAc. The combined extracts were dried and concentrated to give a brown oil. Purification by flash chromatography (eluent 10% MeOH/CH2Cl2) gave a yellow oil 1.47 g (77%).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 20 hours
  3. concentrationThe mixture was concentrated
  4. additiondiluted with H2O
  5. extractionextracted with EtOAc
  6. customThe combined extracts were dried
  7. concentrationconcentrated
  8. customto give a brown oil
  9. customPurification by flash chromatography (eluent 10% MeOH/CH2Cl2)

出典と根拠

ORDレコード
ord-7321103da4424e62b67272e0136ebb39
出典データセット
uspto-grants-1992_09
特許番号
US05149700

反応ノート

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