Dibenz(b,f)azepine → Carbamazepine

HRID 1744396

반응식

HRID 1744396 반응식
[CH:1]1[CH:2]=[CH:3][C:4]2[NH:15][C:14]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=3[CH:8]=[CH:7][C:5]=2[CH:6]=1.[O-:16][C:17]#[N:18].[Na+]>C(O)(=O)C.C(O)C>[CH:1]1[CH:2]=[CH:3][C:4]2[N:15]([C:17]([NH2:18])=[O:16])[C:14]3[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=3[CH:8]=[CH:7][C:5]=2[CH:6]=1

참가 물질

5

반응물 2

HCID 9212Dibenz(b,f)azepineHCID 517096Sodium Cyanate

생성물 1

HCID 2554Carbamazepine수율 80.3%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

30 g iminostilbene are heated to 60° C. in 360 ml acetic acid and 50 ml ethanol, and 20 g 98% sodium cyanate is added within 1.5 hours at this temperature. After a short heating to 80° C., the mixture is further stirred at 60° C., and then cooled to 15° C., sucked off, washed with 20 l acetic acid and dried to yield 29.4 g (80.3% of theoretical) of carbamazepine, having a melting point of 189° C. to 192° C.

후처리

  1. temperaturecooled to 15° C.
  2. washwashed with 20 l acetic acid
  3. customdried

출처 및 근거

ORD 기록
ord-25819033458c4515bfe6d3a3aa574b2d
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07015322B1

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