Allyltributylstannane → Benzene, 4-nitro-1-(2-propen-1-yl)-2-(trifluoromethyl)-

HRID 1466120

반응식

HRID 1466120 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[C:11]([F:14])([F:13])[F:12].[CH2:15]([Sn](CCCC)(CCCC)CCCC)[CH:16]=[CH2:17].[Cl-].[Li+]>C1(C)C=CC=CC=1.C(OCC)(=O)C.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>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([CH2:17][CH:16]=[CH2:15])=[C:3]([C:11]([F:14])([F:13])[F:12])[CH:4]=1)([O-:10])=[O:9]

참가 물질

7

반응물 3

HCID 90628AllyltributylstannaneHCID 1361982-Bromo-5-nitrobenzotrifluorideHCID 433294Lithium Chloride

생성물 1

HCID 9816036Benzene, 4-nitro-1-(2-propen-1-yl)-2-(trifluoromethyl)-

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매HCID 1140Toluene용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 1-bromo-4-nitro-2-(trifluoromethyl)benzene (1.0 g, 3.7 mmol), Allyl Tri-n-butyltin (1.4 mL, 4.4 mmol), Lithium Chloride (470 mg, 11 mmol), and Palladium Tetrakis (210 mg, 0.18 mmol) in toluene (30 mL) was heated to reflux for 16 hours under nitrogen. TLC showed complete reaction at that point. The reaction was diluted with ethyl acetate, adsorbed onto silica gel, and purified by silica gel chromatography to afford the title product.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 16 hours under nitrogen
  3. customreaction at that point
  4. custompurified by silica gel chromatography

출처 및 근거

ORD 기록
ord-7f88ea31ffa94c30b451d58c8701fb8c
출처 데이터셋
uspto-grants-2015_04
특허 번호
US08999990B2

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