Hydrochloric Acid → HCID 19876799, 화합물

HRID 1886040노트

반응식

HRID 1886040 반응식
[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

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 19876826HCID 19876826, 화합물

생성물 1

HCID 19876799HCID 19876799, 화합물수율 77.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-7321103da4424e62b67272e0136ebb39
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05149700

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