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1,1'-Carbonyldiimidazole → HCID 57991920, 화합물

HRID 2075333
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HRID 2075333 반응식
[Cl:1][C:2]1[CH:7]=[N:6][CH:5]=[C:4]2[S:8][C:9]([C:11]([OH:13])=O)=[CH:10][C:3]=12.C1N=CN(C(N2C=NC=C2)=O)C=1.[NH2:26][NH:27][C:28]([NH2:30])=[S:29]>CN(C=O)C>[Cl:1][C:2]1[CH:7]=[N:6][CH:5]=[C:4]2[S:8][C:9]([C:11]([NH:26][NH:27][C:28]([NH2:30])=[S:29])=[O:13])=[CH:10][C:3]=12
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참가 물질

5

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HCID 682631,1'-CarbonyldiimidazoleHCID 2723789ThiosemicarbazideHCID 185161084-Chlorothieno[2,3-c]pyridine-2-carboxylic acid

생성물 1

HCID 57991920HCID 57991920, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
70 °C

실험 절차

4-Chlorothieno[2,3-c]pyridine-2-carboxylic acid (4.2 g, 19.7 mmol) was dissolved in 110 mL DMF in a round bottom flask. To this flask was added CDI (7.68 g, 47.4 mmol). After the flask was heated at 70° C. for 30 minutes, thiosemicarbazide (4.32 g, 47.4 mmol) dissolved in 5 mL DMF was added and the resulting mixture was heated at 70° C. for 30 minutes. After removing the DMF under reduced pressure, the remaining residue was mixed with 50 mL 1N HCl. After filtration and washing with water, the product was dried in a vacuum oven at 80° C. for 4 hours. The resulting product (6.0 g) was used directly in the next step. LCMS (API-ES) m/z (%): 287.1 (100%, M++H).

후처리

  1. additionwas added
  2. temperaturethe resulting mixture was heated at 70° C. for 30 minutes
  3. customAfter removing the DMF under reduced pressure
  4. additionthe remaining residue was mixed with 50 mL 1N HCl
  5. filtrationAfter filtration
  6. washwashing with water
  7. customthe product was dried in a vacuum oven at 80° C. for 4 hours

출처 및 근거

ORD 기록
ord-037c22bdd4e64189ad0595131106d543
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07919504B2

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