Hydrazine hydrate (1:1) → HCID 69381849, 화합물

HRID 524349노트

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HRID 524349 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][C:19]=1[S:20]([CH3:23])(=[O:22])=[O:21])[CH2:5][N:6]1C(=O)C2C(=CC=CC=2)C1=O.O.NN>CO.ClCCl>[F:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][C:19]=1[S:20]([CH3:23])(=[O:22])=[O:21])[CH2:5][NH2:6]

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 867116022-(3-Fluoro-4-methylsulfonyl-benzyl)-isoindole-1,3-dione

생성물 1

HCID 69381849HCID 69381849, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

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온도
60 °C

실험 절차

The purified intermediate 2-(3-fluoro-4-methylsulfonyl-benzyl)-isoindole-1,3-dione (5.50 g, 15.6 mmol) is dissolved in a mixture of methanol (250 mL) and dichloromethane (250 mL). Hydrazine hydrate (4.6 g, 78.4 mmol) is added, and the mixture is stirred at 60° C. for 3 h. The mixture is filtered, and the filtrate is treated with water. The mixture is extracted with ethyl acetate, and the organic layer is dried over Na2SO4 and concentrated under reduced pressure. The residue is purified by preparative reversed-phase HPLC (Luna C18 250*50 mm, gradient of acetonitrile in water, 0.1% TFA). Yield: 3.1 g (81% of theory); ESI mass spectrum: [M+H]+=204; Retention time HPLC: 0.17 min (X012_S01).

후처리

  1. filtrationThe mixture is filtered
  2. additionthe filtrate is treated with water
  3. extractionThe mixture is extracted with ethyl acetate
  4. dry with materialthe organic layer is dried over Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customThe residue is purified by preparative reversed-phase HPLC (Luna C18 250*50 mm, gradient of acetonitrile in water, 0.1% TFA)
  7. custom0.17 min (X012_S01)

출처 및 근거

ORD 기록
ord-b8e9dfaf4230490382e25d375f1dac02
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340507B2

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