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Sodium Hydroxide → (3-Bromo-5-pyrazol-1-yl-phenyl)-thiourea

HRID 1010646
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HRID 1010646 반응식
[OH-].[Na+].C([NH:11][C:12]([NH:14][C:15]1[CH:20]=[C:19]([N:21]2[CH:25]=[CH:24][CH:23]=[N:22]2)[CH:18]=[C:17]([Br:26])[CH:16]=1)=[S:13])(=O)C1C=CC=CC=1>O.C1COCC1>[Br:26][C:17]1[CH:16]=[C:15]([NH:14][C:12]([NH2:11])=[S:13])[CH:20]=[C:19]([N:21]2[CH:25]=[CH:24][CH:23]=[N:22]2)[CH:18]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 57813664HCID 57813664, 화합물

생성물 1

HCID 57813577(3-Bromo-5-pyrazol-1-yl-phenyl)-thiourea수율 85.4%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

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온도
70 °C

실험 절차

A solution of NaOH (0.13 g, 3.35 mmol) dissolved in 1.0 mL of H2O was added to a solution of 1-Benzoyl-3-(3-bromo-5-pyrazol-1-yl-phenyl)-thiourea 3 (0.27 g, 0.67 mmol) in 5.0 mL of THF. The resulting reaction mixture was stirred at 70° C. for 12 hours. THF was distilled off and extracted with ethyl acetate (×3). The combined organic layer was dried over Na2SO4, filtered and distilled off to get the crude residue that was washed with 2% Ethyl acetate-hexane to obtain the desired compound (0.17 g, 85%).

후처리

  1. customThe resulting reaction mixture
  2. distillationTHF was distilled off
  3. extractionextracted with ethyl acetate (×3)
  4. dry with materialThe combined organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. distillationdistilled off
  7. customto get the crude residue that
  8. washwas washed with 2% Ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-dabe82ff76774a88b75dfc7a34881ee0
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07977340B2

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