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Dimethylformamide → 3-(3-Isopentylthio-1,2,5-thiadiazol-4-yl)-1-azabicyclo[2.2.2]octane fumarate

HRID 651452
ノート
印刷プレビュー

反応式

HRID 651452 の反応式
Cl[C:2]1[C:6]([CH:7]2[CH:12]3[CH2:13][CH2:14][N:9]([CH2:10][CH2:11]3)[CH2:8]2)=[N:5][S:4][N:3]=1.[OH2:15].[SH2:16].[Na].[C:18](=[O:21])([O-:20])[O-].[K+].[K+].Br[CH2:25][CH2:26][CH:27]([CH3:29])[CH3:28].CN([CH:33]=[O:34])C>O>[C:33]([OH:34])(=[O:15])/[CH:13]=[CH:14]/[C:18]([OH:20])=[O:21].[CH2:25]([S:16][C:2]1[C:6]([CH:7]2[CH:12]3[CH2:13][CH2:14][N:9]([CH2:10][CH2:11]3)[CH2:8]2)=[N:5][S:4][N:3]=1)[CH2:26][CH:27]([CH3:29])[CH3:28]
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 6228Dimethylformamide2 回HCID 78911-Bromo-3-methylbutaneHCID 11430Potassium CarbonateHCID 99427073-Chloro-4-quinuclidin-3-yl-1,2,5-thiadiazole2 回HCID 53442613Sodium hydrogen sulfide hydrate

生成物 1

HCID 217086333-(3-Isopentylthio-1,2,5-thiadiazol-4-yl)-1-azabicyclo[2.2.2]octane fumarate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 3-(3-chloro-1,2,5-thiadiazol-4-yl)-1-azabicyclo[2.2.2]octane (Compound 8) (420 mg, 1.83 mmol), sodiumhydrogen sulfide monohydrate (245 mg, 3.70 mmol) and potassium carbonate (780 mg, 5.64 mmol) in DMF (20 ml) was stirred at room temperature for 2 h. A solution of 1-bromo-3-methylbutane (420 mg, 2.75 mmol) in DMF (5 ml) was added, and the reaction mixture was stirred at room temperature for 3 h. Water (20 ml) was added and the mixture was extracted with ethyl acetate (3×100 ml). The combined extract was washed with brine, dried (MgSO4), filtered and evaporated. The residue was purified by column chromatography (eluent: CH2Cl2:MeOH:NH4OH (8:2:0.5%)) to give the free base of the desired product in 400 mg yield. Crystallization of the residue with fumaric acid from isopropanol/ether gave the title compound in 370 mg yield. (Compound 99). M.p. 130-132° C.

後処理

  1. extractionthe mixture was extracted with ethyl acetate (3×100 ml)
  2. extractionThe combined extract
  3. washwas washed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified by column chromatography (eluent: CH2Cl2:MeOH:NH4OH (8:2:0.5%))

出典と根拠

ORDレコード
ord-979b133ce82b42068898e039222813a9
出典データセット
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06281233B1

反応ノート

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