Sodium Bicarbonate → HCID 59557741、化合物

HRID 2038478ノート

反応式

HRID 2038478 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:17])=[C:6]([CH:16]=1)[CH2:7][C:8]1[CH:15]=[CH:14][C:11]([CH:12]=O)=[CH:10][CH:9]=1.[C:18]([O-])(O)=O.[Na+]>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:17])=[C:6]([CH2:7][C:8]2[CH:15]=[CH:14][C:11]([CH:12]=[CH2:18])=[CH:10][CH:9]=2)[CH:16]=1

参加物

4

反応物 2

HCID 516892Sodium BicarbonateHCID 59557754HCID 59557754、化合物

生成物 1

HCID 59557741HCID 59557741、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

To a solution of Ph3PCH3I (0.97 g) in toluene (5 mL), KN(TMS)2 (0.5M in toluene, 4.8 mL) was added dropwise at room temperature. After 10 min, the solution of 4-(5-bromo-2-chlorobenzyl)benzaldehyde (intermediate AL) (0.62 g) in toluene (2 mL) was added dropwise. After 2 h, aqueous NaHCO3 was added to quench the reaction, and the resulting mixture was extracted with ethyl acetate. The organic layers were combined, washed with brine, and dried over Na2SO4. The solvent was evaporated under reduced pressure, and the product was purified by column chromatography to obtain pure intermediate AM (0.5 g).

後処理

  1. waitAfter 2 h
  2. customto quench
  3. customthe reaction
  4. extractionthe resulting mixture was extracted with ethyl acetate
  5. washwashed with brine
  6. dry with materialdried over Na2SO4
  7. customThe solvent was evaporated under reduced pressure
  8. customthe product was purified by column chromatography
  9. customto obtain pure intermediate

出典と根拠

ORDレコード
ord-fc11bfeb9fac49d1812034dd9905e9f7
出典データセット
uspto-grants-2013_11
特許番号
US08575321B2

反応ノート

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