Nitromethane → 1H-benzimidazol-1-ol 3-oxide

HRID 1607719

반응식

HRID 1607719 반응식
[N+]([CH3:4])([O-])=O.[CH:5]1[CH:13]=[CH:12][C:11]2[C:7](=[N:8][O:9][N+:10]=2[O-:14])[CH:6]=1.CC1N=CN=C(C)C=1>O1CCCC1>[OH:9][N:8]1[C:7]2[CH:6]=[CH:5][CH:13]=[CH:12][C:11]=2[N+:10]([O-:14])=[CH:4]1

참가 물질

5

반응물 3

HCID 6375NitromethaneHCID 152574,6-DimethylpyrimidineHCID 68075Benzofuroxan

생성물 1

HCID 123493471H-benzimidazol-1-ol 3-oxide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture containing nitromethane (7.4 g., 0.12 moles), benzofuroxan 13.6 g., 0.10 moles) and tetrahydrofuran (50 ml.) is slowly added dimethylpyrimidine (11.3 g.) dropwise. The heat of reaction causes the reaction temperature to rise sharply; therefore, an ice-bath is used to maintain a steady rate of reflux. Upon completion of addition, the resulting mixture is allowed to cool to room temperature whereupon the solid product which precipitates is filtered, washed with water, dried and recrystallized from a MeOH/NaOCH3 mixture which is subsequently acidified. The crystalline product has an M.P. 213° C. dec.

후처리

  1. temperatureThe heat of reaction
  2. customtherefore, an ice-bath is used
  3. temperatureto maintain a steady rate
  4. temperatureof reflux
  5. additionUpon completion of addition
  6. customprecipitates
  7. filtrationis filtered
  8. washwashed with water
  9. customdried
  10. customrecrystallized from a MeOH/NaOCH3 mixture which

출처 및 근거

ORD 기록
ord-7e53e56e1e234f45b968485bf6b00ec8
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04866175

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