Potassium Carbonate → HCID 178508870、化合物

HRID 1014931ノート

反応式

HRID 1014931 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 178508870HCID 178508870、化合物収率 68.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-e935b28794954a5990241555437b808b
出典データセット
uspto-grants-2011_07
特許番号
US07985745B2

反応ノート

読み込み中…