Nitric Acid → HCID 178494273、化合物

HRID 345426ノート

反応式

HRID 345426 の反応式
[N+:1]([O-:4])(O)=[O:2].[OH:5][C:6]1[CH:11]=[C:10]([OH:12])[N:9]=[C:8]([O:13][CH3:14])[N:7]=1>CC(O)=O>[OH:5][C:6]1[C:11]([N+:1]([O-:4])=[O:2])=[C:10]([OH:12])[N:9]=[C:8]([O:13][CH3:14])[N:7]=1

参加物

4

反応物 2

HCID 944Nitric AcidHCID 178494256HCID 178494256、化合物

生成物 1

HCID 178494273HCID 178494273、化合物収率 68%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To glacial HOAc (860 mL) was added red fuming HNO3 (300 mL) with cooling and stirring, at such a rate that the temperature was kept below 20° C. This stirred mixture was cooled in an ice bath and the foregoing material prepared in Example 134 (200 g, 78% pure, 1.1 mol) was added in portions over a period of 1 hr such that the temperature was maintained between 18°-20° C. The reaction was then stirred overnight. The precipitate which formed was filtered off and washed with HOAc (50 mL). This solid was then slurried with ice-H2O (400 mL), filtered off and dried to constant weight in vacuo at 60° C. to yield 141 g (0.75 mol, 68% yield) of the title compound; nmr (d6 -DMSO) d: 3.95 (s); mass spectrum showed m/e 187 (M+). A separate synthesis gave an analytical sample.

後処理

  1. temperaturewith cooling
  2. customwas kept below 20° C
  3. temperatureThis stirred mixture was cooled in an ice bath
  4. temperaturewas maintained between 18°-20° C
  5. stirringThe reaction was then stirred overnight
  6. customThe precipitate which formed
  7. filtrationwas filtered off
  8. washwashed with HOAc (50 mL)
  9. filtrationfiltered off
  10. customdried to constant weight in vacuo at 60° C.

出典と根拠

ORDレコード
ord-c4419a069d704a05847f68787c78033e
出典データセット
uspto-grants-1991_10
特許番号
US05057517

反応ノート

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