Ethyl Acetate → HCID 21476295、化合物

HRID 2293099ノート

反応式

HRID 2293099 の反応式
C(OCC)(=O)C.Br.[NH2:8][CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:19]3[CH:20]=[CH:21][C:22](=[O:25])[NH:23][N:24]=3)[CH:16]=2)[CH2:11]1.C(=O)([O-])[O-].[Na+].[Na+].[CH2:32]([S:34](Cl)(=[O:36])=[O:35])[CH3:33]>O1CCCC1>[CH2:32]([S:34]([NH:8][CH2:9][CH:10]1[CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:19]3[CH:20]=[CH:21][C:22](=[O:25])[NH:23][N:24]=3)[CH:16]=2)[CH2:11]1)(=[O:36])=[O:35])[CH3:33]

参加物

6

反応物 4

HCID 8857Ethyl Acetate2 回HCID 10340Sodium CarbonateHCID 11667Ethanesulfonyl chlorideHCID 214762912-aminomethyl-5-[pyridazin-3(2H)-on-6-yl]indane hydrobromide

生成物 1

HCID 21476295HCID 21476295、化合物収率 82.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

In a mixed solution of 30 ml of ethyl acetate and 30 ml of tetrahydrofuran was suspended 3.22 g of 2-aminomethyl-5-[pyridazin-3(2H)-on-6-yl]indane hydrobromide. A sodium carbonate aqueous solution (5.30 g/30 ml of water) was added to the suspension. Under ice cooling, 3.32 g of ethanesulfonyl chloride dissolved in 10 ml of tetrahydrofuran was added to the mixture, and the resulting mixture was stirred for 3 hours. 300 ml of ethyl acetate was added to the mixture. After the organic layer was collected by separation, washed with water and dried, and the solvent was removed. The residue was purified by silica gel column chromatography (chloroform-methanol (100:3)) to obtain 2.75 g of 2-(ethylsulfonylaminomethyl)-5-[pyridazin-3(2H)-on-6-yl]indane.

後処理

  1. additionwas added to the mixture
  2. customAfter the organic layer was collected by separation
  3. washwashed with water
  4. customdried
  5. customthe solvent was removed
  6. customThe residue was purified by silica gel column chromatography (chloroform-methanol (100:3))

出典と根拠

ORDレコード
ord-3c61e454e9b64a54b7055d90cbe2b4f2
出典データセット
uspto-grants-1997_11
特許番号
US05686452

反応ノート

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