1-Butyne → 2-But-1-ynyl-5-fluoro-phenylamine

HRID 1640247

반응식

HRID 1640247 반응식
[CH2:1]1[CH2:5]O[CH2:3][CH2:2]1.[F:6][C:7]1[CH:8]=[CH:9][C:10](I)=[C:11]([CH:13]=1)[NH2:12].C(N(CC)CC)C.C#CCC>C(OCC)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Cu](I)I>[C:5]([C:10]1[CH:9]=[CH:8][C:7]([F:6])=[CH:13][C:11]=1[NH2:12])#[C:1][CH2:2][CH3:3]

참가 물질

8

반응물 4

HCID 78461-ButyneHCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 27745125-Fluoro-2-iodoaniline

생성물 1

HCID 581174762-But-1-ynyl-5-fluoro-phenylamine

시약·촉매·용매 3

HCID 83717Copper iodide촉매HCID 178418476HCID 178418476, 화합물촉매HCID 3283Diethyl Ether용매

실험 절차

160 mL of THF were placed in the flask and degassed with argon. Then 10 g (45 mmol) 5-fluoro-2-iodo-aniline, 1.5 g (2.1 mmol) PdCl2(PPh3)2 and 0.40 g (2.1 mmol) copper iodide were added and the flask was rinsed with argon. Then 18 mL (0.13 mol) triethylamine were added and 3.0 g (55 mmol) 1-butyne (in gaseous form) were passed through the solution. The reaction mixture was stirred for 3 h at RT, then diluted with diethyl ether, filtered through kieselguhr and evaporated down.

후처리

  1. customdegassed with argon
  2. washthe flask was rinsed with argon
  3. filtrationfiltered through kieselguhr
  4. customevaporated down

출처 및 근거

ORD 기록
ord-db4a19ae8e89483987734dd1bd3132c5
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110575B2

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