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Potassium Hydroxide → 3-bromo-2-methyl-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazole

HRID 1909058
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반응식

HRID 1909058 반응식
[Br:1][C:2]1[C:3]([CH3:11])=[N:4][NH:5][C:6]=1[CH2:7][CH2:8][CH2:9]Cl.[OH-].[K+]>C(O)(C)C.O>[Br:1][C:2]1[C:3]([CH3:11])=[N:4][N:5]2[CH2:9][CH2:8][CH2:7][C:6]=12
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참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 178434607HCID 178434607, 화합물

생성물 1

HCID 665994623-bromo-2-methyl-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazole수율 49%

시약·촉매·용매 2

HCID 962Water용매HCID 3776Isopropanol용매

실험 절차

To a solution of 4-bromo-5-(3-chloro-propyl)-3-methyl-1H-pyrazole (2.42 g, 10.2 mmol) in isopropyl alcohol (35 mL) was added KOH (0.86 g, 15.3 mmol) dissolved in water (7 mL). The reaction was heated to reflux for 4 h. After cooling the reaction was partially concentrated, diluted with EtOAc and washed with brine. The organic layer was dried over Na2SO4, filtered and concentrated to give a light yellow oil as the desired product (1.01 g, 5.0 mmol). MS m/z 203.4 (M+H)+.

후처리

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 4 h
  3. temperatureAfter cooling the reaction
  4. concentrationwas partially concentrated
  5. additiondiluted with EtOAc
  6. washwashed with brine
  7. dry with materialThe organic layer was dried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-afe1c77df44c433591b865d1cdc7202e
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598217B2

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