Acetic Acid → HCID 14402879、化合物

HRID 1381825ノート

反応式

HRID 1381825 の反応式
C(O)(=O)C.O.[C:6]([CH2:8][N:9]1[C:14]2[CH:15]=[C:16]([N+:19]([O-])=O)[CH:17]=[CH:18][C:13]=2[O:12][CH2:11][C:10]1=[O:22])#[N:7]>[Fe].C(O)C>[NH2:19][C:16]1[CH:17]=[CH:18][C:13]2[O:12][CH2:11][C:10](=[O:22])[N:9]([CH2:8][C:6]#[N:7])[C:14]=2[CH:15]=1

参加物

6

反応物 3

HCID 176Acetic AcidHCID 962WaterHCID 14402878HCID 14402878、化合物

生成物 1

HCID 14402879HCID 14402879、化合物収率 74.4%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒2 回

反応条件

温度
80 °C

実験手順

A mixture of ethanol (15 ml), acetic acid (1 g), water (25 ml) and iron (3 g) is stirred at 80° C., and 4-cyanomethyl-6-nitro-2H-1,4-benzoxazin-3(4H)-one (2.33 g) is added portionwise thereto. The whole is stirred at 80° C. until gas evolution ceases. The reaction mixture is mixed with active carbon (1 g) and ethanol (20 ml), refluxed for 15 minutes, and filtered. The filtrate is poured into chilled water. The deposited crystals are collected by filtration, and dried to obtain 6-amino-4-cyanomethyl-2H-1,4-benzoxazin-3(4H)-one (1.51 g).

後処理

  1. stirringThe whole is stirred at 80° C. until gas evolution ceases
  2. temperaturerefluxed for 15 minutes
  3. filtrationfiltered
  4. additionThe filtrate is poured
  5. temperatureinto chilled water
  6. filtrationThe deposited crystals are collected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-715ca77a502248729df48cda7b5786db
出典データセット
uspto-grants-1989_02
特許番号
US04804394

反応ノート

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