Ammonia → 6-Chloro-2-methylpyrimidine-4,5-diamine

HRID 339794

반응식

HRID 339794 반응식
[NH2:1][C:2]1[C:3](Cl)=[N:4][C:5]([CH3:9])=[N:6][C:7]=1[Cl:8].[NH3:11]>C(O)(C)C>[Cl:8][C:7]1[N:6]=[C:5]([CH3:9])[N:4]=[C:3]([NH2:11])[C:2]=1[NH2:1]

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 7366744,6-Dichloro-2-methylpyrimidin-5-amine

생성물 1

HCID 5941456-Chloro-2-methylpyrimidine-4,5-diamine수율 91%

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
150 °C

실험 절차

A 200 mL stainless steel Parr vessel was loaded with 5-amino-4,6-dichloro-2-methylpyrimidine (7.2 g, 40 mmol) and 2 M ammonia in isopropanol (100 mL), and then was sealed and heated at 150° C. for 16 h. HPLC analysis indicated complete conversion. The mixture was concentrated in vacuo, and the residue was suspended in a mixture of H2O (10 mL) and isopropanol (35 mL). This was stirred at 50° C. for 1 h and then was cooled to room temperature. The precipitate was collected by suction filtration, washed sparingly with isopropanol, then air dried on the filter to afford 6-chloro-4,5-diamino-2-methylpyrimidine (5.8 g, 91%) as a brown powder, which was used without further purification in the next step.

후처리

  1. customwas sealed
  2. concentrationThe mixture was concentrated in vacuo
  3. additionthe residue was suspended in a mixture of H2O (10 mL) and isopropanol (35 mL)
  4. temperaturewas cooled to room temperature
  5. filtrationThe precipitate was collected by suction filtration
  6. washwashed sparingly with isopropanol
  7. customair dried on the
  8. filtrationfilter

출처 및 근거

ORD 기록
ord-e243258ad81a4b0185dda7b3f4dc6261
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895568B2

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