Formic Acid → 4-Oxo-4H-chromene-3-carbonitrile

HRID 1578611

反応式

HRID 1578611 の反応式
[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][CH:4]=[C:3]1[CH:12]=O.Cl.[NH2:15]O.C([O-])=O.[Na+].C(O)=O>O>[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][CH:4]=[C:3]1[C:12]#[N:15]

参加物

6

反応物 4

HCID 284Formic AcidHCID 871123-FormylchromoneHCID 443297Hydroxyamine hydrochlorideHCID 2723810Sodium Formate

生成物 1

HCID 5212984-Oxo-4H-chromene-3-carbonitrile

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 26.1 g. (0.15 mole) of 4-oxo-4H-1-benzopyran-3-carboxaldehyde, 13.1 g. (0.19 mole) of hydroxylamine hydrochloride, 18.4 g. (0.27 mole) of sodium formate and 250 ml of 99% formic acid was heated with stirring at reflux for 21/2 hours. Water was added to 1-liter volume. The separated solid was filtered from the cooled mixture, washed well with water and dried to give 13 g. (51%) of crude nitrile melting at 138°-145°C. Recrystallization from ethylacetate gave pure, white crystals melting at 174°-176°.

後処理

  1. additionA mixture of 26.1 g
  2. temperatureat reflux for 21/2 hours
  3. filtrationThe separated solid was filtered from the cooled mixture
  4. washwashed well with water
  5. customdried
  6. customto give 13 g
  7. customRecrystallization from ethylacetate
  8. customgave pure

出典と根拠

ORDレコード
ord-374965f0f83b449f936ea6acdee65858
出典データセット
uspto-grants-1976_02
特許番号
US03937837

関連ノート

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