Acetic Acid → HCID 14402879, 화합물

HRID 1381825노트

반응식

HRID 1381825 반응식
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

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 962WaterHCID 14402878HCID 14402878, 화합물

생성물 1

HCID 14402879HCID 14402879, 화합물수율 74.4%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 702Ethanol용매2회

반응 조건

온도
80 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-715ca77a502248729df48cda7b5786db
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04804394

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