1,1'-Carbonyldiimidazole → HCID 68536364, 화합물

HRID 2374688노트

반응식

HRID 2374688 반응식
[O:1]1[CH2:6][CH2:5][CH2:4][O:3][CH:2]1[C:7]1[CH:15]=[CH:14][C:10]([C:11](O)=O)=[C:9]([F:16])[CH:8]=1.C(N1C=CN=C1)(N1C=CN=C1)=O.Cl.Cl.[NH2:31][C:32]1[C:40]([NH2:41])=[CH:39][CH:38]=[CH:37][C:33]=1[C:34]([NH2:36])=[O:35]>N1C=CC=CC=1.CN(C=O)C>[O:1]1[CH2:6][CH2:5][CH2:4][O:3][CH:2]1[C:7]1[CH:15]=[CH:14][C:10]([C:11]2[NH:41][C:40]3[CH:39]=[CH:38][CH:37]=[C:33]([C:34]([NH2:36])=[O:35])[C:32]=3[N:31]=2)=[C:9]([F:16])[CH:8]=1

참가 물질

6

반응물 3

HCID 682631,1'-CarbonyldiimidazoleHCID 534228072,3-Diaminobenzamide dihydrochlorideHCID 68533538HCID 68533538, 화합물

생성물 1

HCID 68536364HCID 68536364, 화합물수율 50%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6228Dimethylformamide용매

실험 절차

A solution of EXAMPLE 22B (770 mg, 3.4 mmol) in pyridine (5 mL) and N,N′-dimethylformamide (10 mL) was treated with 1,1′-carbonyldiimidazole (763 mg, 3.4 mmol) at 40° C. for 30 minutes. 2,3-Diaminobenzamide dihydrochloride (826 mg, 5.1 mmol) was added and the mixture stirred at ambient temperature overnight. The mixture was concentrated and the residue refluxed overnight in 20 mL of xylene and 2 mL of acetic acid. After cooling and concentration, the residue was purified by flash chromatography on silica gel using ethyl acetate to give the title compound (550 mg, 50%). MS (DCI/NH3) m/z 342 (M+H)+.

후처리

  1. concentrationThe mixture was concentrated
  2. temperaturethe residue refluxed overnight in 20 mL of xylene
  3. temperatureAfter cooling
  4. concentrationconcentration
  5. customthe residue was purified by flash chromatography on silica gel

출처 및 근거

ORD 기록
ord-9b5e666957904556822f3929a1ac302d
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07462724B2

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