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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Lawesson's reagent → HCID 86643630, 화합물

HRID 2061868
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HRID 2061868 반응식
[Br:1][C:2]1[C:3]([C:16](=O)[NH2:17])=[CH:4][C:5]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[N:6][CH:7]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:28])=CC=1>O1CCCC1>[Br:1][C:2]1[C:3]([C:16](=[S:28])[NH2:17])=[CH:4][C:5]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[N:6][CH:7]=1
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참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 67029027HCID 67029027, 화합물2회

생성물 1

HCID 86643630HCID 86643630, 화합물수율 97.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The crude tert-butyl 5-bromo-4-carbamoylpyridin-2-ylcarbamate (Intermediate 84, 232 mmol) was treated with Lawesson's Reagent (94 g, 232 mmol, 1 eq) and tetrahydrofuran (700 mL), the resulting mixture was heated at reflux for 1 h, then it was allowed to stir at room temperature over the weekend. The mixture was concentrated to dryness in vacuo and toluene (˜300 mL) was added. A bright yellow solid precipitated formed which was collected by filtration and washed with toluene, then dried in the vacuum oven at 50° C. for 4 h, yielding 75 g of a bright yellow solid (97%).

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureat reflux for 1 h
  3. concentrationThe mixture was concentrated to dryness in vacuo and toluene (˜300 mL)
  4. additionwas added
  5. customA bright yellow solid precipitated
  6. customformed which
  7. filtrationwas collected by filtration
  8. washwashed with toluene
  9. customdried in the vacuum oven at 50° C. for 4 h

출처 및 근거

ORD 기록
ord-7ee22519fe2d4c7293ab9e4725767b91
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08283361B2

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