Sodium Hydroxide → HCID 59557754, 화합물

HRID 425043노트

반응식

HRID 425043 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:17])=[C:6]([CH:16]=1)[CH2:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][OH:15])=[CH:10][CH:9]=1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.[OH-].[Na+]>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([Cl:17])=[C:6]([CH:16]=1)[CH2:7][C:8]1[CH:13]=[CH:12][C:11]([CH:14]=[O:15])=[CH:10][CH:9]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 159087TriacetoxyperiodinaneHCID 59557735HCID 59557735, 화합물

생성물 1

HCID 59557754HCID 59557754, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To a solution of (4-(5-bromo-2-chlorobenzyl)phenyl)methanol (intermediate AK) (1 g) in CH2Cl2 (10 mL), the solution of Dess-Martin periodinane (DMP) (1.22 g) in CH2Cl2 (10 mL) was added dropwise at 0° C. The mixture was warmed to room temperature, and the reaction was monitored by TLC. After 1 h, CH2Cl2 was added to dilute the solution and 1 M NaOH was added to quench the reaction. The CH2Cl2 layer was separated and washed with aqueous NaHSO3 and brine, and dried over Na2SO4. The solvent was evaporated under reduced pressure, and the product was purified by column chromatography to obtain pure intermediate AL (0.62 g).

후처리

  1. additionwas added
  2. customto quench
  3. customthe reaction
  4. customThe CH2Cl2 layer was separated
  5. washwashed with aqueous NaHSO3 and 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 AL (0.62 g)

출처 및 근거

ORD 기록
ord-6163956b4c224c2fbd01ed681a1f8c9f
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08106021B2

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