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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sodium Iodide → N-((4aS,7aS)-7a-(5-Amino-2-fluorophenyl)-4a,5,7,7a-tetrahydro-4H-furo[3,4-d][1,3]thiazin-2-yl)benzamide

HRID 2060755
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인쇄 미리보기

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HRID 2060755 반응식
Br[C:2]1[CH:3]=[CH:4][C:5]([F:26])=[C:6]([C@:8]23[CH2:16][O:15][CH2:14][C@H:13]2[CH2:12][S:11][C:10]([NH:17][C:18](=[O:25])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[N:9]3)[CH:7]=1.FC(F)(F)C([NH2:31])=O.[I-].[Na+].C(=O)([O-])[O-].[K+].[K+].[C@@H]1(N)CCCC[C@H]1N>[Cu]I.O.CO>[NH2:31][C:2]1[CH:3]=[CH:4][C:5]([F:26])=[C:6]([C@:8]23[CH2:16][O:15][CH2:14][C@H:13]2[CH2:12][S:11][C:10]([NH:17][C:18](=[O:25])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[N:9]3)[CH:7]=1
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참가 물질

9

반응물 5

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 438061,2-Diaminocyclohexane, trans-HCID 67717TrifluoroacetamideHCID 57504885HCID 57504885, 화합물

생성물 1

HCID 57504887N-((4aS,7aS)-7a-(5-Amino-2-fluorophenyl)-4a,5,7,7a-tetrahydro-4H-furo[3,4-d][1,3]thiazin-2-yl)benzamide
수율 49.9%

시약·촉매·용매 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매HCID 887Methanol용매HCID 962Water용매

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온도
22 °C

실험 절차

To a 2 L round bottom flask is added N-((4aS,7aS)-7a-(5-bromo-2-fluorophenyl)-4a,5,7,7a-tetrahydro-4H-furo[3,4-d][1,3]thiazin-2-yl)benzamide (35.0 g, 80.4 mmol), trifluoroacetamide (16.2 g, 143 mmol), copper(I) iodide (2.66 g, 13.7 mmol), sodium iodide (21.3 g, 141 mmol) and potassium carbonate (21.5 g, 153 mmol). The flask is capped with a septum, vacuum and back filled with nitrogen. 1,4-dioxane (731 mL) (previously degassed with vacuum-nitrogen) is added via cannula, and N,N′-dimethyl-, trans (+/−) 1,2-cyclohexanediamine (10.1 g, 70.8 mmol) is added. The mixture is placed in a preheated oil bath at 100° C. and stirred at this temperature for 19 h. The septum is replaced by a reflux condenser and a mixture of methanol (154 mL) and water (154 mL) is added through the condenser. The mixture is stirred at 100° C. for 3.5 h, cooled to 22° C., and concentrated partially under reduced pressure (to 0.6 L volume). Aqueous ammonium hydroxide (25%, 154 mL) is added and the mixture is stirred for 10 min. The mixture is extracted three times with ethyl acetate (3×500 mL) and the solvent is removed under reduced pressure. A residue is obtained that is purified by flash chromatography with a linear gradient of 50% to 75% ethyl acetate in hexane to give the title compound (14.9 g, 47%). ES/MS m/e: 372 (M+1).

후처리

  1. customThe flask is capped with a septum, vacuum
  2. additionback filled with nitrogen
  3. custom1,4-dioxane (731 mL) (previously degassed with vacuum-nitrogen)
  4. additionis added
  5. customThe mixture is placed in a preheated oil bath at 100° C.
  6. customThe septum is replaced by a reflux condenser
  7. additionis added through the condenser
  8. stirringThe mixture is stirred at 100° C. for 3.5 h
  9. concentrationconcentrated partially under reduced pressure (to 0.6 L volume)
  10. additionAqueous ammonium hydroxide (25%, 154 mL) is added
  11. stirringthe mixture is stirred for 10 min
  12. extractionThe mixture is extracted three times with ethyl acetate (3×500 mL)
  13. customthe solvent is removed under reduced pressure
  14. customA residue is obtained
  15. customthat is purified by flash chromatography with a linear gradient of 50% to 75% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-cadae58793e44ec5a256aafea856697c
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08278441B2

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