Triethylamine → HCID 23435529, 화합물

HRID 860078

반응식

HRID 860078 반응식
Cl[C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.Cl.[CH2:11]([NH2:13])[CH3:12].CCN(CC)CC>C(O)CCC>[NH2:8][C:6]1[CH:5]=[C:4]([Cl:9])[N:3]=[C:2]([NH:13][CH2:11][CH3:12])[N:7]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 11198Ethylamine hydrochlorideHCID 823874-Pyrimidinamine, 2,6-dichloro-

생성물 1

HCID 23435529HCID 23435529, 화합물

시약·촉매·용매 1

HCID 2631-Butanol용매

반응 조건

온도
90 °C

실험 절차

A mixture of 2,6-dichloro-4-aminopyrimidine 18-1 (Avocado; 4.8 g, 29.3 mmol), ethylamine hydrochloride (7.0 g, 85.8 mmol), Et3N (20 mL, 144 mmol) and n-butanol (150 mL) was heated to 90° C. for 6 hours. After cooling, the solvent was removed in vacuo and the residue partitioned between saturated Na2CO3 solution and EtOAc. The EtOAc layer was washed with brine, dried (MgSO4) and concentrated to give an orange solid. Purification by column chromatography (EtOAc/hexane 1:1) gave the title compound 18-2 as a white solid.

후처리

  1. temperatureAfter cooling
  2. customthe solvent was removed in vacuo
  3. customthe residue partitioned between saturated Na2CO3 solution and EtOAc
  4. washThe EtOAc layer was washed with brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customto give an orange solid
  8. customPurification by column chromatography (EtOAc/hexane 1:1)

출처 및 근거

ORD 기록
ord-f375066a496849a29a18fbc735d95bb3
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07153862B2

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