Ammonium Chloride → 1-(2'-(Benzyloxy)-3'-tert-butylbiphenyl-3-yl)-1-(2-methoxyphenyl)ethanol

HRID 45474

반응식

HRID 45474 반응식
[CH2:1]([O:8][C:9]1[C:14]([C:15]([CH3:18])([CH3:17])[CH3:16])=[CH:13][CH:12]=[CH:11][C:10]=1[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25](=[O:27])[CH3:26])[CH:20]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:28][O:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=1[Mg]Br.[Cl-].[NH4+]>O1CCCC1>[CH2:1]([O:8][C:9]1[C:14]([C:15]([CH3:18])([CH3:17])[CH3:16])=[CH:13][CH:12]=[CH:11][C:10]=1[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=2[O:29][CH3:28])([OH:27])[CH3:26])[CH:20]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 582385981-(2'-(Benzyloxy)-3'-tert-butylbiphenyl-3-yl)ethanoneHCID 178489560HCID 178489560, 화합물

생성물 1

HCID 582385991-(2'-(Benzyloxy)-3'-tert-butylbiphenyl-3-yl)-1-(2-methoxyphenyl)ethanol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 36 (0.8 g, 2.23 mmol) in anhydrous tetrahydrofuran (8 mL) was stirred under nitrogen at room temperature and 1M ortho-methoxyphenyl magnesium bromide in tetrahydrofuran (3 mL, 1.35 equiv.) was slowly added. Stirring was continued at room temperature for 30 min and at 60° C. for 3 hr. After cooling, the reaction mixture was poured on saturated ammonium chloride (120 mL) and extracted with ethyl acetate (150 mL). The organic extract was washed with water (2×50 mL), dried over sodium sulfate and filtered. The solvent was removed in a rotary evaporator and the crude 37 thus obtained was used in the next step without further purification.

후처리

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate (150 mL)
  3. extractionThe organic extract
  4. washwas washed with water (2×50 mL)
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customThe solvent was removed in a rotary evaporator
  8. customthe crude 37 thus obtained
  9. customwas used in the next step without further purification

출처 및 근거

ORD 기록
ord-d0dbe5b4edf345aa848c9fad3f26678e
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541522B2

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