Potassium Carbonate → HCID 178508870, 화합물

HRID 1014931노트

반응식

HRID 1014931 반응식
O=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][CH2:5][CH2:4][CH:3]1[C:13]([O:15]C)=O.[Cl-].[NH2:18][C:19]([NH2:21])=[NH:20].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[NH2:21][C:19]1[N:18]=[C:13]([OH:15])[C:3]2[CH2:4][CH2:5][CH2:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[C:2]=2[N:20]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 10104791methyl 5-oxo-6,7,8,9-tetrahydro-5H-benzo[7]annulene-6-carboxylateHCID 21864146CID 21864146

생성물 1

HCID 178508870HCID 178508870, 화합물수율 68.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of the product from Example 4A (4.2 g, est. 18 mmol), guanidine chloride (7.1 g, 72.8 mmol), and K2CO3 (10.8 g, 78 mmol) in DMF (30 mL) was heated to 125° C. for 3 hours. The mixture was cooled and the solids were removed by filtration. The solids were washed with EtOAc. The combined filtrates were concentrated under reduced pressure and the residue was passed through silica gel pad eluting with EtOAc:hexanes (8:2) and then with MeOH:EtOAc:CH2Cl2 (10:45:45) to provide the title compound as a white solid (2.8 g).

후처리

  1. temperatureThe mixture was cooled
  2. customthe solids were removed by filtration
  3. washThe solids were washed with EtOAc
  4. concentrationThe combined filtrates were concentrated under reduced pressure
  5. washeluting with EtOAc:hexanes (8:2)

출처 및 근거

ORD 기록
ord-e935b28794954a5990241555437b808b
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07985745B2

반응 노트

불러오는 중…