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Tris(1,1-dimethylethyl)phosphine → HCID 25006742, 화합물

HRID 2239501
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HRID 2239501 반응식
Br[C:2]1[C:7]([F:8])=[CH:6][C:5]([S:9]([NH:12][CH2:13][CH:14]2[CH2:16][CH2:15]2)(=[O:11])=[O:10])=[C:4]([F:17])[CH:3]=1.[C:18]([C:20]1[N:24]([CH3:25])[C:23](B(O)O)=[CH:22][CH:21]=1)#[N:19].[F-].[K+].C(P(C(C)(C)C)C(C)(C)C)(C)(C)C>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[C:18]([C:20]1[N:24]([CH3:25])[C:23]([C:2]2[C:7]([F:8])=[CH:6][C:5]([S:9]([NH:12][CH2:13][CH:14]3[CH2:16][CH2:15]3)(=[O:11])=[O:10])=[C:4]([F:17])[CH:3]=2)=[CH:22][CH:21]=1)#[N:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 83681Tris(1,1-dimethylethyl)phosphineHCID 522689Potassium FluorideHCID 11708078(5-cyano-1-methyl-1H-pyrrol-2-yl)boronic acidHCID 68482433Benzenesulfonamide, 4-bromo-N-(cyclopropylmethyl)-2,5-difluoro-

생성물 1

HCID 25006742HCID 25006742, 화합물수율 26.8%

시약·촉매·용매 1

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매

실험 절차

According to general procedure B, 4-bromo-N-(cyclopropylmethyl)-2,5-difluorobenzenesulfonamide (150 mg, 0.5 mmol), 5-cyano-1-methyl-1H-pyrrol-2-ylboronic acid (90 mg, 0.60 mmol), potassium fluoride (96 mg, 1.65 mmol), and tris(dibenzylideneacetone)dipalladium (12 mg, 0.013 mmol) were placed in an oven dried flask under nitrogen and dry THF (1.3 mL) was added. Tri-t-butylphosphine (75 μL, 0.026 mmol, 10 wt % in hexane) was added and the reaction was stirred for 16 hours. Purification afforded 4-(5-cyano-1-methyl-1H-pyrrol-2-yl)-N-(cyclopropylmethyl)-2,5-difluorobenzenesulfonamide (47 mg). HPLC purity 98.2% at 210-370 nm, 9.5 min.; the Xterra® RP18 column, 3.5μ, 150×4.6 mm column, 1.2 mL/min., 85/15-5/95 (ammonium formate buffer pH=3.5/ACN+MeOH) for 10 min., hold 4 min. HRMS: calcd for C16H15F2N3O2S−H+, 350.07803; found (ESI-FTMS, [M−H]1−), 350.07826

후처리

  1. customwere placed in an oven
  2. customdried flask under nitrogen
  3. additiondry THF (1.3 mL) was added
  4. customPurification

출처 및 근거

ORD 기록
ord-2048167462d54e08974f0ad71cc99d58
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07723332B2

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