Hydrochloric Acid → HCID 86597347, 화합물

HRID 2117623노트

반응식

HRID 2117623 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[O:11][CH:12]([F:14])[F:13].[C:15]1([OH:21])[CH:20]=CC=C[CH:16]=1.[NH:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1.[C:28](=[O:31])([O-])[O-].[K+].[K+].Cl.[OH-].[Na+].[CH3:37]S(C)=O>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.O>[F:13][CH:12]([F:14])[O:11][C:3]1[CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:7][C:2]=1[N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1.[F:13][CH:12]([F:14])[O:11][C:3]1[CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:7][C:2]=1[N:22]1[CH2:27][CH2:26][N:25]([C:28]([O:21][C:15]([CH3:16])([CH3:20])[CH3:37])=[O:31])[CH2:24][CH2:23]1

참가 물질

10

반응물 7

HCID 313Hydrochloric AcidHCID 679Dimethyl SulfoxideHCID 996PhenolHCID 4837PiperazineHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 534159044-Bromo-3-(difluoromethoxy)nitrobenzene

생성물 1

HCID 86597347HCID 86597347, 화합물

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 962Water용매

실험 절차

A stirred mixture of 1-bromo-2-difluoromethoxy-4-nitrobenzene (prepared from the corresponding phenol following the procedure outlined in WO9749710A1; 2.68 g, 10 mmol), piperazine (1.12 g, 13 mmol), potassium carbonate (2.07 g, 15 mmol), tetrabutylammonium bromide (0.03 g, 0.1 mmol) and dry dimethyl sulphoxide (20 mL) was heated under nitrogen at 120° C. for 3 h. The product was added to water (100 mL) and 6M hydrochloric acid (10 mL, 60 mmol), washed with ethyl acetate until washings colourless and the aqueous layer basified with 5M sodium hydroxide solution (20 mL, 100 mmol). Extraction with ethyl acetate (3× with 50 mL), drying (sodium sulphate) and evaporating gave product as viscous orange oil.

후처리

  1. washwashed with ethyl acetate until washings colourless
  2. extractionExtraction with ethyl acetate (3× with 50 mL)
  3. dry with materialdrying (sodium sulphate)
  4. customevaporating
  5. customgave product as viscous orange oil

출처 및 근거

ORD 기록
ord-fdffdfc0c8cb49cdbff0694c7a1ff046
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07442698B2

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