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Citric Acid → N-Butyloxycarbonyl-3-[3-(2-chloroimidazol-1-ylmethyl)phenyl]-5-iso-butyl-thiophene-2-sulfonamide

HRID 659687
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HRID 659687 반응식
Br[C:2]1[N:3]([CH2:7][C:8]2[CH:9]=[C:10]([C:14]3[CH:18]=[C:17]([CH2:19][CH:20]([CH3:22])[CH3:21])[S:16][C:15]=3[S:23]([NH:26]C(C)(C)C)(=[O:25])=[O:24])[CH:11]=[CH:12][CH:13]=2)[CH:4]=[CH:5][N:6]=1.C1(OC)C=CC=CC=1.N1(C2C=CC=CN=2)[CH2:43][CH2:42][CH2:41][CH2:40]1.[Cl:50]C(OCCCC)=O.C(O)(=O)CC(CC(O)=O)([C:62]([OH:64])=[O:63])O>C(O)(C(F)(F)F)=O>[CH2:40]([O:64][C:62]([NH:26][S:23]([C:15]1[S:16][C:17]([CH2:19][CH:20]([CH3:21])[CH3:22])=[CH:18][C:14]=1[C:10]1[CH:11]=[CH:12][CH:13]=[C:8]([CH2:7][N:3]2[CH:4]=[CH:5][N:6]=[C:2]2[Cl:50])[CH:9]=1)(=[O:24])=[O:25])=[O:63])[CH2:41][CH2:42][CH3:43]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 311Citric AcidHCID 7519AnisoleHCID 61140Butyl chloroformateHCID 110190202-(Pyrrolidin-1-yl)pyridineHCID 671329713-[3-(2-bromoimidazol-1-ylmethyl)phenyl]-5-iso-butyl-N-tert-butylthiophene-2-sulfonamide

생성물 1

HCID 56964911
N-Butyloxycarbonyl-3-[3-(2-chloroimidazol-1-ylmethyl)phenyl]-5-iso-butyl-thiophene-2-sulfonamide
수율 57%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

To a solution of 3-[3-(2-bromoimidazol-1-ylmethyl)phenyl]-5-iso-butyl-N-tert-butylthiophene-2-sulfonamide (44.1 mg, 0.086 mmol; see step (b)) in TFA (3 mL) was added anisole (150 μL) and the reaction mixture was stirred overnight at ambient temperature. The reaction mixture was concentrated in vacuo and dried in vacuo overnight. To the crude product dissolved in pyridine (1.5 mL) was added pyrrolidinopyridine (25.6 mg, 0.173 mmol) and butyl chloroformate (109.9 μL, 0.846 mmol) and the reaction mixture was stirred for 36 h. Citric acid (3 mL, 10% aq) was added to the reaction mixture, which was then extracted with EtOAc, dried (over anhydrous MgSO4), concentrated in vacuo, and the residue purified by flash chromatography using MeOH:CH2Cl2 (5:95) as eluent to give the title compound in 57% yield, over two steps, (25 mg, 0.049 mmol).

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customdried in vacuo overnight
  3. dissolutionTo the crude product dissolved in pyridine (1.5 mL)
  4. stirringthe reaction mixture was stirred for 36 h
  5. extractionwas then extracted with EtOAc
  6. dry with materialdried (over anhydrous MgSO4)
  7. concentrationconcentrated in vacuo
  8. customthe residue purified by flash chromatography

출처 및 근거

ORD 기록
ord-c6456d65e9af4a6eaea292b86fe50fa9
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08080571B2

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