HCID 66889465, 화합물 → HCID 49854331, 화합물

HRID 1895548노트

반응식

HRID 1895548 반응식
[NH2:1][C:2]1[C:7]([C:8](=[O:10])[NH2:9])=[CH:6][CH:5]=[CH:4][C:3]=1[NH:11][C:12]([CH:14]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH2:17][CH2:16][N:15]1[C:24]([O:26][CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)=[O:25])=O>C(O)(=O)C>[C:8]([C:7]1[C:2]2[N:1]=[C:12]([CH:14]3[C:23]4[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=4)[CH2:17][CH2:16][N:15]3[C:24]([O:26][CH2:27][C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)=[O:25])[NH:11][C:3]=2[CH:4]=[CH:5][CH:6]=1)(=[O:10])[NH2:9]

참가 물질

3

반응물 1

HCID 66889465HCID 66889465, 화합물

생성물 1

HCID 49854331HCID 49854331, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Step-2: A solution of benzyl 1-((2-amino-3-carbamoylphenyl)carbamoyl)-3,4-dihydroisoquinoline-2(1H)-carboxylate (425 mg, 0.956 mmol) in acetic acid (5 ml) was heated to 80° C. and stirred overnight. The reaction mixture was concentrated, neutralized with aq. NaHCO3 and extracted with DCM. The DCM layer was washed with brine, dried over anhydrous sodium sulfate and evaporated. Purification of the crude product over silica gel column using ethyl acetate/hexane mixture (1:1) as eluent afforded benzyl 1-(4-carbamoyl-1H-benzo[d]imidazol-2-yl)-3,4-dihydroisoquinoline-2(1H)-carboxylate. MS (ES+): m/z 427.2 [M+H]+

후처리

  1. concentrationThe reaction mixture was concentrated
  2. extractionextracted with DCM
  3. washThe DCM layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated
  6. customPurification of the crude product over silica gel column

출처 및 근거

ORD 기록
ord-f4fe45a302064e5bbc24b209af664550
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08513433B2

반응 노트

불러오는 중…