Water → HCID 66820102、化合物

HRID 1044789ノート

反応式

HRID 1044789 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 66820102HCID 66820102、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
55 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9c9d4931848d466ca076fad9b4a3ab7c
出典データセット
uspto-grants-2013_10
特許番号
US08563714B2

反応ノート

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