Hydrochloric Acid → HCID 22631480、化合物

HRID 1840434ノート

反応式

HRID 1840434 の反応式
[N:1]([CH2:4][CH2:5][CH2:6][S:7][C:8]1[N:9]=[CH:10][N:11]2[CH:15]=[CH:14][S:13][C:12]=12)=[N+]=[N-].Cl.[H][H]>C1COCC1.C(O)C.O.[Pd]>[NH2:1][CH2:4][CH2:5][CH2:6][S:7][C:8]1[N:9]=[CH:10][N:11]2[CH:15]=[CH:14][S:13][C:12]=12

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 22631922HCID 22631922、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 22631480HCID 22631480、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 962Water溶媒HCID 21873804Tetrahydrofuran ethanol溶媒

実験手順

7-(3-Azidopropyl)thioimidazo[5,1-b]thiazole (1.46 g) was dissolved in 30 ml of THF ethanol and 6 ml of water, and 6.1 ml of a 1 N aqueous hydrochloric acid solution and 1.46 g of 10% Pd-C were added to the solution. The air in the reaction vessel was replaced by hydrogen, and the contents of the reaction vessel were stirred at room temperature for 24 hr. The catalyst was removed by filtration on Celite, and was washed with water. The filtrate was concentrated under the reduced pressure. A 1 N aqueous sodium hydroxide solution (20 ml) was added to the residue, and the mixture was extracted with dichloromethane five times. The extract was dried over anhydrous magnesium sulfate. The solvent was removed by distillation to prepare 1.15 g of 7-(3-aminopropyl)thioimidazo[5,1-b]thiazole.

後処理

  1. customThe catalyst was removed by filtration on Celite
  2. washwas washed with water
  3. concentrationThe filtrate was concentrated under the reduced pressure
  4. additionA 1 N aqueous sodium hydroxide solution (20 ml) was added to the residue
  5. extractionthe mixture was extracted with dichloromethane five times
  6. dry with materialThe extract was dried over anhydrous magnesium sulfate
  7. customThe solvent was removed by distillation
  8. customto prepare 1.15 g of 7-(3-aminopropyl)thioimidazo[5,1-b]thiazole

出典と根拠

ORDレコード
ord-7ab91ee2e1cd441e83bcba9f88e7a2c9
出典データセット
uspto-grants-2004_01
特許番号
US06680313B2

反応ノート

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