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1-Iodohexane → HCID 67401054, 화합물

HRID 906640
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HRID 906640 반응식
[OH:1][CH:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.CCN(C(C)C)[CH:11]([CH3:13])[CH3:12].ClC1C=[CH:22][C:21]([C:24]([NH:26][CH2:27][C:28]2[S:32][C:31]([S:33](Cl)(=[O:35])=[O:34])=[CH:30][CH:29]=2)=O)=CC=1.[H-].[Na+].I[CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH3:45]>C(Cl)Cl.ClCCCl.CN(C=O)C.CCOC(C)=O>[CH2:13]([N:26]([CH2:24][CH:21]=[CH2:22])[CH2:27][C:28]1[S:32][C:31]([S:33]([N:5]2[CH2:6][CH2:7][CH:2]([O:1][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH3:45])[CH2:3][CH2:4]2)(=[O:34])=[O:35])=[CH:30][CH:29]=1)[CH:11]=[CH2:12]
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참가 물질

10

반응물 5

HCID 125271-IodohexaneHCID 24758Sodium hydrideHCID 79341Piperidin-4-olHCID 81531DiisopropylethylamineHCID 27357135-((4-Chlorobenzamido)methyl)thiophene-2-sulfonyl chloride

생성물 1

HCID 67401054HCID 67401054, 화합물

시약·촉매·용매 4

HCID 11
1,2-Dichloroethane
용매
HCID 6228Dimethylformamide용매
HCID 6344Dichloromethane용매
HCID 8857Ethyl Acetate용매

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온도
70 °C

실험 절차

To a solution of 4-hydroxy-piperidine (190 mg, 1.88 mmol) and DIEA (0.87 mL, 5.13 mmol) in 10 mL CH2Cl2 was added a solution of 5-({[1-(4-Chloro-phenyl)-methanoyl]-amino}-methyl)-thiophene-2-sulfonyl chloride 1b (500 mg, 1.71 mmol) in hot DCE. The reaction mixture was stirred for 4 h. 100 mL EtOAc were added and excess of amines were removed by extraction with HCl (1N). The sulfonamide intermediate was used without any further purification, where 300 mg (0.84 mmol) were dissolved in dry DMF under Ar. NaH (60 mg, 50% in parafine oil, 1.01 mmol) were added as a solid. The colour of the reaction changed to orange. The reaction mixture was stirred for 15′ until no gas evolution was observed anymore. Iodohexane (356 mg, 1.68 mmol) dissolved in 1 mL DMF was added to the above solution and the reaction mixture was heated at 70° C. overnight. DMF was evaporated to dryness and the crude was taken up in CH2Cl2. The organic layer was washed twice with water, dried over MgSO4 and evaporated to dryness. The crude was purified on silica gel using cyclohexane/EtOAc 3:1 as eluent to obtain 210 mg (59%) of pure 326a as a colorless oil.

후처리

  1. customwere removed by extraction with HCl (1N)
  2. customThe sulfonamide intermediate was used without any further purification, where 300 mg (0.84 mmol)
  3. dissolutionwere dissolved in dry DMF under Ar
  4. stirringThe reaction mixture was stirred for 15′ until no gas evolution
  5. additionwas added to the above solution
  6. customDMF was evaporated to dryness
  7. washThe organic layer was washed twice with water
  8. dry with materialdried over MgSO4
  9. customevaporated to dryness
  10. customThe crude was purified on silica gel

출처 및 근거

ORD 기록
ord-5f5d8992766e4071981ca8bd53312e04
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08012995B1

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