Water → 2-acryloylamino-5-[pyridazin-3(2H)-on-6-yl]indane

HRID 1077427노트

반응식

HRID 1077427 반응식
[C:1](Cl)(=[O:4])[CH:2]=[CH2:3].[NH2:6][CH:7]1[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[C:12]([C:16]3[CH:17]=[CH:18][C:19](=[O:22])[NH:20][N:21]=3)[CH:13]=2)[CH2:8]1.Br.O.C(=O)([O-])[O-].[K+].[K+]>O1CCCC1.C(OCC)(=O)C>[C:1]([NH:6][CH:7]1[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[C:12]([C:16]3[CH:17]=[CH:18][C:19](=[O:22])[NH:20][N:21]=3)[CH:13]=2)[CH2:8]1)(=[O:4])[CH:2]=[CH2:3]

참가 물질

7

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 13140Acryloyl chlorideHCID 189297722-amino-5-[pyridazin-3(2H)-on-6-yl]indane hydrobromide

생성물 1

HCID 199728542-acryloylamino-5-[pyridazin-3(2H)-on-6-yl]indane수율 80.4%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

Under ice cooling, 3.0 g of acryloyl chloride dissolved in 50 ml of tetrahydrofuran was added dropwise to a suspension of 5.03 g of 2-amino-5-[pyridazin-3(2H)-on-6-yl]indane·hydrobromide in 150 ml of ethyl acetate and 150 ml of water containing 4.52 g of potassium carbonate, and the mixture was stirred for 3 hours. Crystals precipitated were collected by filtration, washed with water, dried and then recrystallized from methanol-acetonitrile to obtain 3.69 g of 2-acryloylamino-5-[pyridazin-3(2H)-on-6-yl]indane.

후처리

  1. customCrystals precipitated
  2. filtrationwere collected by filtration
  3. washwashed with water
  4. customdried
  5. customrecrystallized from methanol-acetonitrile

출처 및 근거

ORD 기록
ord-99af5a186c2e40ba956f8123a329b311
출처 데이터셋
uspto-grants-1996_08
특허 번호
US05543409

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