O-Xylene → HCID 178507852, 화합물

HRID 27225

반응식

HRID 27225 반응식
[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH2:9])[CH:5]=[C:4](Cl)[N:3]=1.CC1C=CC=CC=1C.[NH:19]1[CH2:24][CH2:23][CH:22]=[CH:21][CH2:20]1.[OH-].[Na+]>O>[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH2:9])[CH:5]=[C:4]([N:19]2[CH2:20][CH:21]=[CH:22][CH2:23][CH2:24]2)[N:3]=1

참가 물질

6

반응물 4

HCID 7237O-XyleneHCID 127501,2,3,6-TetrahydropyridineHCID 14798Sodium HydroxideHCID 178507684HCID 178507684, 화합물

생성물 1

HCID 178507852HCID 178507852, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
5 °C

실험 절차

155 g. of 2,4-diamino-6-chloropyrimidine-3-oxide are mixed and stirred under an argon atmosphere with 640 ml. of o-xylene and 260 ml. of 1,2,5,6-tetrahydropyridine. The mixture is then heated to reflux for 30 minutes, the internal temperature rising from 115° C. to 123° C. The mixture is then cooled to 5° C., treated with 40 g. of sodium hydroxide in 400 ml. of water and stirred at 5° C. for 1 hour. The precipitate formed is filtered off, washed with 200 ml. of water and recrystallized from 3000 ml. of water, there being obtained pure 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide having a melting point of 263°-265° C. (decomposition).

후처리

  1. temperatureThe mixture is then heated
  2. temperatureto reflux for 30 minutes
  3. customrising from 115° C. to 123° C
  4. additiontreated with 40 g
  5. customThe precipitate formed
  6. filtrationis filtered off
  7. washwashed with 200 ml
  8. customof water and recrystallized from 3000 ml

출처 및 근거

ORD 기록
ord-78235fc49efa4141bd34f86d567c32f7
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04220772

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