Sodium Hydroxide → HCID 59557754, 화합물

HRID 2403720노트

반응식

HRID 2403720 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 6344Dichloromethane용매2회

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) CH2Cl2 (10 mL) was added dropwise. 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. custom0° C
  2. additionwas added
  3. customto quench
  4. customthe reaction
  5. customThe CH2Cl2 layer was separated
  6. washwashed with aqueous NaHSO3 and brine
  7. dry with materialdried over Na2SO4
  8. customThe solvent was evaporated under reduced pressure
  9. customthe product was purified by column chromatography
  10. customto obtain pure intermediate AL (0.62 g)

출처 및 근거

ORD 기록
ord-ab345eeaf99c410697f63be67e99949c
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802637B2

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