Ammonia → RO-05-2921

HRID 1973067

반응식

HRID 1973067 반응식
C(O)C.C1N2CN3CN(C2)C[N:5]1C3.N.Cl[CH2:16][C:17]([NH:19][C:20]1[CH:33]=[CH:32][CH:31]=[CH:30][C:21]=1[C:22]([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)=O)=[O:18]>C(Cl)(Cl)Cl>[C:24]1([C:22]2[C:21]3[CH:30]=[CH:31][CH:32]=[CH:33][C:20]=3[NH:19][C:17](=[O:18])[CH2:16][N:5]=2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

6

반응물 4

HCID 222Ammonia2회HCID 702EthanolHCID 4101HexamethylenetetramineHCID 2064069N-(2-benzoylphenyl)-2-chloroacetamide

생성물 1

HCID 76175RO-05-2921수율 86%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of ethanol (300 ml) and hexamethylenetetramine (20 g., 0.143 mol) was stirred, heated to reflux, and saturated with ammonia. 2-Chloroacetamidobenzophenone (18.1 g., 0.066 mol) was added in small increments over 3 to 4 hours while a steady stream of ammonia was bubbled into the reaction mixture. Refluxing was continued for 3 hours after complete addition of 2-chloroacetamidobenzophenone. The flow of ammonia was interrupted and the ethanol removed by distillation in vacuo. The residue obtained was taken up in chloroform (200 ml), and washed with water (100 ml) at 50° C. The chloroform layer was evaporated to dryness at 30° C. and the oily solid obtained was recrystallized from toluene (100 ml) to give 1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one (13.2 g., 86%), melting at 184°-186° C.

후처리

  1. temperatureheated
  2. temperatureto reflux
  3. customwas bubbled into the reaction mixture
  4. temperatureRefluxing
  5. additionafter complete addition of 2-chloroacetamidobenzophenone
  6. customthe ethanol removed by distillation in vacuo
  7. customThe residue obtained
  8. washwashed with water (100 ml) at 50° C
  9. customThe chloroform layer was evaporated to dryness at 30° C.
  10. customthe oily solid obtained
  11. customwas recrystallized from toluene (100 ml)

출처 및 근거

ORD 기록
ord-a8b74999058a436a995fac845a405bd5
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03996209

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