Sodium Hydroxide → HCID 68862086, 화합물

HRID 871195

반응식

HRID 871195 반응식
[Br:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([Br:10])[C:3]=1[CH:4]=[O:5].[CH:11](O)([OH:14])[CH2:12][CH3:13].C(OC(OCC)OCC)C.[OH-].[Na+]>C(Cl)Cl.[Cl-].[Cl-].[Cl-].[Cl-].[Zr+4]>[Br:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([Br:10])[C:3]=1[CH:4]1[O:14][CH2:11][CH2:12][CH2:13][O:5]1

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 31214Ethyl orthoformateHCID 134919PropanediolHCID 126486412,6-Dibromobenzaldehyde

생성물 1

HCID 68862086HCID 68862086, 화합물수율 98%

시약·촉매·용매 2

HCID 9856075Zirconium chloride (ZrCl4), (T-4)-촉매HCID 6344Dichloromethane용매

실험 절차

2,6-Dibromobenzaldehyde (49) (10.0 g, 37.9 mmol) was dissolved in 160 ml dry CH2Cl2. Propanediol (6.4 ml, 88.5 ml), triethylorthoformate (6.83 ml, 41 mmol) and anhydrous ZrCl4 (1.0 g) were added at ambient temperature and stirred overnight. Then NaOH (50 ml of a 10% solution) was added and stirred for an additional hour. The organic phase was separated, the aqueous phase was extracted with Et2O (2×40 ml). The combined organic phases were washed with water (3×60 ml), dried over MgSO4 and the volatiles were removed in vacuo to afford 12 g (98%) 2-(2,6-Dibromophenyl)-1,3-dioxane (acetal) as a slightly yellow solid.

후처리

  1. stirringstirred for an additional hour
  2. customThe organic phase was separated
  3. extractionthe aqueous phase was extracted with Et2O (2×40 ml)
  4. washThe combined organic phases were washed with water (3×60 ml)
  5. dry with materialdried over MgSO4
  6. customthe volatiles were removed in vacuo

출처 및 근거

ORD 기록
ord-39a49ebe1c9f419c8d447ac9182f1073
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969624B2

연결된 노트

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