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Triethylamine → N-[5-(5-Cyanopyridin-3-ylethynyl)-2-fluorobenzyl]-methanesulfonamide

HRID 606915
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HRID 606915 반응식
C(N(CC)CC)C.Br[C:9]1[CH:10]=[N:11][CH:12]=[C:13]([CH:16]=1)[C:14]#[N:15].[F:17][C:18]1[CH:29]=[CH:28][C:27]([C:30]#[C:31][Si](C)(C)C)=[CH:26][C:19]=1[CH2:20][NH:21][S:22]([CH3:25])(=[O:24])=[O:23].[F-].C([N+](CCCC)(CCCC)CCCC)CCC>O1CCCC1.[Br-].[Zn+2].[Br-].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:14]([C:13]1[CH:16]=[C:9]([C:31]#[C:30][C:27]2[CH:28]=[CH:29][C:18]([F:17])=[C:19]([CH:26]=2)[CH2:20][NH:21][S:22]([CH3:25])(=[O:24])=[O:23])[CH:10]=[N:11][CH:12]=1)#[N:15]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 7367935-BromonicotinonitrileHCID 2724141Tetrabutylammonium Fluoride2회HCID 67047541N-(2-Fluoro-5-trimethylsilanylethynylbenzyl)-methanesulfonamide

생성물 1

HCID 67047961N-[5-(5-Cyanopyridin-3-ylethynyl)-2-fluorobenzyl]-methanesulfonamide수율 50.6%

시약·촉매·용매 3

HCID 10421208
Zinc bromide
촉매
HCID 178418397HCID 178418397, 화합물촉매
HCID 8028Tetrahydrofuran용매3회

반응 조건

온도
60 °C

실험 절차

Dissolve zinc (II) bromide (94 mg, 0.36 mmol) in tetrahydrofuran (0.75 mL) and treat with triethylamine (0.20 mL, 1.4 mmol). After 4 min add 5-bromonicotinonitrile (55 mg, 0.30 mmol), N-(2-fluoro-5-trimethylsilanylethynylbenzyl) -methanesulfonamide, (prepared as described in PREPARATION 34), (100 mg, 0.33 mmol) and tetrakis(triphenylphosphine)palladium (0) (17 mg, 0.015 mmol) to the reddish solution. Heat to 60° C. and add a 1 M solution of tetrabutylammonium fluoride (0.36 mL) in tetrahydrofuran. After 1 h add additional 1 M tetrabutylammonium fluoride (0.3 mL) in tetrahydrofuran and stir an additional 30 min. Cool to room temperature and filter through diatomaceous earth washing with ethyl acetate. Purify by silica gel chromatography, eluting with a gradient from 60:40 to 40:60 (7:30 hexanes:dichloromethane):ethyl acetate, to give the title compound as a white crystalline solid (50 mg, 50%).

후처리

  1. temperatureCool to room temperature
  2. filtrationfilter through diatomaceous earth
  3. washwashing with ethyl acetate
  4. customPurify by silica gel chromatography
  5. washeluting with a gradient from 60:40 to 40:60 (7:30 hexanes:dichloromethane)

출처 및 근거

ORD 기록
ord-54630c9503d6492ba83d33c0591b1825
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07915424B2

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