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1,1'-Carbonyldiimidazole → HCID 86636675, 화합물

HRID 2075391
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HRID 2075391 반응식
[F:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][C:8]([C:12]([OH:14])=O)=[CH:7][CH:6]=2.N1(C(N2C=CN=C2)=O)C=CN=C1.[NH2:27][NH:28][C:29]([NH2:31])=[S:30]>CN(C=O)C>[F:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[CH:9][C:8]([C:12]([NH:27][NH:28][C:29]([NH2:31])=[S:30])=[O:14])=[CH:7][CH:6]=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 682631,1'-CarbonyldiimidazoleHCID 2723789ThiosemicarbazideHCID 57991948HCID 57991948, 화합물

생성물 1

HCID 86636675HCID 86636675, 화합물수율 89%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 3-fluoroisoquinoline-6-carboxylic acid (0.71 g, 3.72 mmol) and di(1H-imidazol-1-yl)methanone (1.21 g, 7.44 mmol) in DMF (9.0 mL) was stirred at room temperature for 1 hour and 20 minutes until no gas was evolved. The reaction mixture was heated at 70° C. for 40 minutes. Thiosemicarbazide (1.02 g, 11.2 mmol) was added, and the reaction mixture was stirred at 70° C. for another 30 minutes. The solvents were removed under reduced pressure. HCl (1.0 N, 50 mL) was added, and the solids were recovered by filtration, and washed with water to provide the product as an off-white solid (0.86 g, 89%). LCMS (API-ES) m/z: 265 (M+H+).

후처리

  1. temperatureThe reaction mixture was heated at 70° C. for 40 minutes
  2. stirringthe reaction mixture was stirred at 70° C. for another 30 minutes
  3. customThe solvents were removed under reduced pressure
  4. additionHCl (1.0 N, 50 mL) was added
  5. filtrationthe solids were recovered by filtration
  6. washwashed with water

출처 및 근거

ORD 기록
ord-58a54495633c45f79e5a27cb056eb974
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07919504B2

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