Tetrahydrofuran → HCID 22989337、化合物

HRID 1169139ノート

反応式

HRID 1169139 の反応式
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][NH:6][C:7]([C:9]1[N:10]=[C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[N:13][N:12]2[CH:18]=1)=[O:8])[CH3:2].[Cl:20]N1C(=O)CCC1=O.O1CCCC1>C(OCC)(=O)C>[CH2:1]([O:3][C:4](=[O:19])[CH2:5][NH:6][C:7]([C:9]1[N:10]=[C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[N:13][N:12]2[C:18]=1[Cl:20])=[O:8])[CH3:2]

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 31398ChlorosuccinimideHCID 22989255N-(6-chloroimidazo-[1,2-b]pyridazine-2-carbonyl)glycine ethyl ester

生成物 1

HCID 22989337HCID 22989337、化合物収率 57.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

0.86 g of N-(6-Chloroimidazo[1,2-b]pyridazine-2-carbonyl)glycine ethyl ester was suspended in 30 ml of ethyl acetate; 1.2 g of N-chlorosuccinimide was added, followed by thermal refluxing for 20 hours. After cooling, 30 ml of tetrahydrofuran was added; the mixture was washed with an aqueous solution of sodium thiosulfate and saline, dried over magnesium sulfate and concentrated under reduced pressure; ethyl ether was added to the residue; the crystal precipitated was collected by filtration, washed with ethyl ether and dried to yield 0.552 g of the title compound.

後処理

  1. customrefluxing for 20 hours
  2. temperatureAfter cooling
  3. washthe mixture was washed with an aqueous solution of sodium thiosulfate and saline
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. additionethyl ether was added to the residue
  7. customthe crystal precipitated
  8. filtrationwas collected by filtration
  9. washwashed with ethyl ether
  10. customdried

出典と根拠

ORDレコード
ord-cbfdd4747edc4600a031a6157d66cebb
出典データセット
uspto-grants-2003_09
特許番号
US06627630B1

反応ノート

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