Water → HCID 66820102, 화합물

HRID 1044789노트

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HRID 1044789 반응식
[N:1]([CH2:4][C:5]1[CH:10]=[CH:9][C:8]([Br:11])=[C:7]([F:12])[C:6]=1[F:13])=[N+]=[N-].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O>C1COCC1>[Br:11][C:8]1[CH:9]=[CH:10][C:5]([CH2:4][NH2:1])=[C:6]([F:13])[C:7]=1[F:12]

참가 물질

5

반응물 3

HCID 962WaterHCID 11776TriphenylphosphineHCID 91256229Benzene, 1-(azidomethyl)-4-bromo-2,3-difluoro-

생성물 1

HCID 66820102HCID 66820102, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
55 °C

실험 절차

To a mixture of the crude azide (164 mg, 0.60 mmol) in THF (3 mL) were added polymer-supported Ph3P (2.0 eq.) and water (1 mL). The reaction mixture was stirred at 55° C. until completion of the reaction, cooled down to rt and filtered. The filtrate was partitioned between EA and aq. sat. NaHCO3 and the layers separated. The aq. layer was extracted with EA and the combined org. extracts dried over MgSO4, filtered and concentrated under reduced pressure to give the title compound as a yellow oil. LC-MS-conditions 07: tR=0.42 min; [M+CH3CN+H]+=263.15.

후처리

  1. temperaturecooled down to rt
  2. filtrationfiltered
  3. customThe filtrate was partitioned between EA and aq. sat. NaHCO3
  4. customthe layers separated
  5. extractionThe aq. layer was extracted with EA
  6. dry with materialextracts dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9c9d4931848d466ca076fad9b4a3ab7c
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08563714B2

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