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Triethylamine → N-(2-Fluoro-5-trimethylsilanylethynylbenzyl)-methanesulfonamide

HRID 606815
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인쇄 미리보기

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HRID 606815 반응식
C(N(CC)CC)C.Br[C:9]1[CH:10]=[CH:11][C:12]([F:21])=[C:13]([CH:20]=1)[CH2:14][NH:15][S:16]([CH3:19])(=[O:18])=[O:17].[CH3:22][Si:23]([C:26]#[CH:27])([CH3:25])[CH3:24]>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>[F:21][C:12]1[CH:11]=[CH:10][C:9]([C:27]#[C:26][Si:23]([CH3:25])([CH3:24])[CH3:22])=[CH:20][C:13]=1[CH2:14][NH:15][S:16]([CH3:19])(=[O:18])=[O:17]
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7

반응물 3

HCID 8471TriethylamineHCID 66111TrimethylsilylacetyleneHCID 40161431N-(5-bromo-2-fluorobenzyl)methanesulfonamide

생성물 1

HCID 67047541N-(2-Fluoro-5-trimethylsilanylethynylbenzyl)-methanesulfonamide수율 74%

시약·촉매·용매 3

HCID 10421208Zinc bromide촉매
HCID 178418397
HCID 178418397, 화합물
촉매
HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

Dissolve zinc (II) bromide (313 mg, 1.20 mmol) in tetrahydrofuran (2.5 mL) and treat with triethylamine (0.64 mL, 4.80 mmol). After 4 min add N-(5-bromo-2-fluorobenzyl)methanesulfonamide (282 mg, 1.00 mmol), (prepared as described in PREPARATION 35), trimethylsilylacetylene (0.30 mL, 2.12 mmol), and tetrakis(triphenylphosphine)palladium (0) (58 mg, 0.050 mmol) to the reddish solution. Heat to 60° C. in a sealed tube overnight, cool to room temperature and filter through diatomaceous earth with ethyl acetate. Concentrate the filtrate and purify the residue by silica gel chromatography, eluting with 75:25 hexanes:ethyl acetate, to give the title compound as a white crystalline solid (220 mg, 74%).

후처리

  1. temperaturecool to room temperature
  2. filtrationfilter through diatomaceous earth with ethyl acetate
  3. concentrationConcentrate the filtrate
  4. custompurify the residue by silica gel chromatography
  5. washeluting with 75:25 hexanes

출처 및 근거

ORD 기록
ord-d2f92a028c4849448d327706acd8e3fe
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07915424B2

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