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Hydrochloric Acid → HCID 135405232, 화합물

HRID 982637
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인쇄 미리보기

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HRID 982637 반응식
B(Br)(Br)Br.[CH3:5][S:6]([C:9]1[CH:14]=[CH:13][C:12]([C:15]2[C:16]([C:24]3[CH:29]=[CH:28][C:27]([O:30]C)=[CH:26][CH:25]=3)=[N:17][N:18]3[C:23]=2[CH:22]=[CH:21][CH:20]=[N:19]3)=[CH:11][CH:10]=1)(=[O:8])=[O:7].C(=O)([O-])[O-].[K+].[K+].Cl>C(Cl)Cl.O>[CH3:5][S:6]([C:9]1[CH:10]=[CH:11][C:12]([C:15]2[C:16]([C:24]3[CH:25]=[CH:26][C:27]([OH:30])=[CH:28][CH:29]=3)=[N:17][N:18]3[C:23]=2[CH:22]=[CH:21][CH:20]=[N:19]3)=[CH:13][CH:14]=1)(=[O:7])=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 25134Boron tribromideHCID 11440364HCID 11440364, 화합물

생성물 1

HCID 135405232HCID 135405232, 화합물수율 54.2%

시약·촉매·용매 2

HCID 962Water용매
HCID 6344
Dichloromethane
용매

실험 절차

Boron tribromide (1M solution in CH2Cl2, 2.1 eq) was added to 3-(4-methanesulfonyl-phenyl)-2-(4-methoxy-phenyl)-pyrazolo[1,5-b]pyridazine (3.58 g) in CH2Cl2 at −70°. The mixture was stirred for 10 min then warmed to 0° and stirred at 0° overnight. The reaction mixture was made alkaline with potassium carbonate then acidified with hydrochloric acid (2M), poured into water and extracted into CH2Cl2. The organic phase was dried, filtered and concentrated to give the title compound (1.87 g) as a yellow solid.

후처리

  1. temperaturethen warmed to 0°
  2. stirringstirred at 0° overnight
  3. extractionextracted into CH2Cl2
  4. customThe organic phase was dried
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-577ace7882584fc79a5bb385977a3600
출처 데이터셋
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06861429B2

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