Sodium Sulfite → HCID 88580856, 화합물

HRID 575524

반응식

HRID 575524 반응식
[Cl:1][C:2]1[N:7]=[C:6]([CH3:8])[N:5]=[C:4]([NH2:9])[CH:3]=1.[I:10]Cl.S([O-])([O-])=O.[Na+].[Na+]>CO>[Cl:1][C:2]1[N:7]=[C:6]([CH3:8])[N:5]=[C:4]([NH2:9])[C:3]=1[I:10]

참가 물질

5

반응물 3

HCID 24437Sodium SulfiteHCID 24640Iodine chlorideHCID 2867546-Chloro-2-methylpyrimidin-4-amine

생성물 1

HCID 88580856HCID 88580856, 화합물수율 80%

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
2.5 °C

실험 절차

Combine 6-chloro-2-methylpyrimidin-4-amine (708 g, 4.93 mol) and MeOH (7.08 L) in a 20 L round bottom flask equipped with a mechanical stirrer. Cool to 0-5° C. Add iodine monochloride (4.806 kg, 29.6 mol) dissolved in MeOH (6 L) using an addition funnel over a period of 1 h. Warm the reaction mixture to RT and stir at RT for 16 h. Cool the reaction mixture to 0-5° C. and add sodium sulfite (46 L, 20% aqueous solution). Filter the resulting solid and wash with water (2 L) followed by hexane (3 L). Dry the solid under vacuum to afford the title compound as a white solid (1061 g, 80%). LC-ES/MS m/z 269.9 (M+1).

후처리

  1. customof 1 h
  2. temperatureWarm the reaction mixture to RT
  3. temperatureCool the reaction mixture to 0-5° C.
  4. filtrationFilter the resulting solid
  5. washwash with water (2 L)
  6. customDry the solid under vacuum

출처 및 근거

ORD 기록
ord-f70f3c19650644a99b8c0b25040f25f2
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09035051B1

연결된 노트

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