Ethyl Acetate → HCID 21476295, 화합물

HRID 2293099노트

반응식

HRID 2293099 반응식
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]

참가 물질

6

반응물 4

HCID 8857Ethyl Acetate2회HCID 10340Sodium CarbonateHCID 11667Ethanesulfonyl chlorideHCID 214762912-aminomethyl-5-[pyridazin-3(2H)-on-6-yl]indane hydrobromide

생성물 1

HCID 21476295HCID 21476295, 화합물수율 82.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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))

출처 및 근거

ORD 기록
ord-3c61e454e9b64a54b7055d90cbe2b4f2
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05686452

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