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

HRID 659687
ノート
印刷プレビュー

反応式

HRID 659687 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c6456d65e9af4a6eaea292b86fe50fa9
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08080571B2

反応ノート

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