3-Bromoaniline → HCID 22225739、化合物

HRID 366510

反応式

HRID 366510 の反応式
[Si:1]([O:8][CH2:9][CH2:10][C:11]#[CH:12])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].Br[C:14]1[CH:15]=[C:16]([CH:18]=[CH:19][CH:20]=1)[NH2:17]>C(N)CCC.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>[O:8]([CH2:9][CH2:10][C:11]#[C:12][C:14]1[CH:20]=[CH:19][CH:18]=[C:16]([NH2:17])[CH:15]=1)[Si:1]([C:4]([CH3:5])([CH3:6])[CH3:7])([CH3:3])[CH3:2]

参加物

5

反応物 2

HCID 115623-BromoanilineHCID 4304567(But-3-yn-1-yloxy)(tert-butyl)dimethylsilane

生成物 1

HCID 22225739HCID 22225739、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 8007Butylamine溶媒

実験手順

A mixture of 1-(t-butyldimethylsilyloxy)-3-butyne (10 mmol) and m-bromoaniline (10 mmol) in n-butylamine (50 mL) under a nitrogen atmosphere is treated with tetrakis(triphenylphosphine)palladium (0) (0.17 g) and then heated to reflux for 18 hr. After removing the solvent in vacuo, the residue is dissolved in CH2Cl2 and washed with saturated NaHCO3. The combined organic solution is dried over magnesium sulfate, filtered and evaporated to give the above described silyl protected adduct.

後処理

  1. temperatureheated
  2. temperatureto reflux for 18 hr
  3. customAfter removing the solvent in vacuo
  4. dissolutionthe residue is dissolved in CH2Cl2
  5. washwashed with saturated NaHCO3
  6. dry with materialThe combined organic solution is dried over magnesium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. customto give the

出典と根拠

ORDレコード
ord-2bffa424f5384ed486a6d8f0e064a4a9
出典データセット
uspto-grants-2000_10
特許番号
US06130234

関連ノート

読み込み中…