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4-Bromo-1,2-dichlorobenzene → 9-(3,4-Dichloro-phenyl)-9-hydroxy-3-aza-spiro[5.5]undecane-3-carboxylic acid tert-butyl ester

HRID 419274
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HRID 419274 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[C:4]([Cl:9])[CH:3]=1.[Li]CCCC.[C:15]([O:19][C:20]([N:22]1[CH2:27][CH2:26][C:25]2([CH2:32][CH2:31][C:30](=[O:33])[CH2:29][CH2:28]2)[CH2:24][CH2:23]1)=[O:21])([CH3:18])([CH3:17])[CH3:16]>C1COCC1>[C:15]([O:19][C:20]([N:22]1[CH2:27][CH2:26][C:25]2([CH2:28][CH2:29][C:30]([C:2]3[CH:7]=[CH:6][C:5]([Cl:8])=[C:4]([Cl:9])[CH:3]=3)([OH:33])[CH2:31][CH2:32]2)[CH2:24][CH2:23]1)=[O:21])([CH3:18])([CH3:16])[CH3:17]
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참가 물질

5

반응물 3

HCID 290134-Bromo-1,2-dichlorobenzeneHCID 51072194tert-Butyl 9-oxo-3-azaspiro[5.5]undecane-3-carboxylateHCID 178418339Butyllithium

생성물 1

HCID 666507759-(3,4-Dichloro-phenyl)-9-hydroxy-3-aza-spiro[5.5]undecane-3-carboxylic acid tert-butyl ester수율 35.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
-78 °C

실험 절차

1-Bromo-3,4-dichlorobenzene (1.35 g, 5.98 mmol) in THF (10 mL) was added drop-wise to a solution of n-BuLi (1.6 M in hexanes, 4 mL) at −78° C. The mixture was stirred for 40 min at −78° C. A solution of 9-oxo-3-aza-spiro[5.5]undecane-3-carboxylic acid tert-butyl ester (1 g, 3.74 mmol) in THF (10 mL) was added drop-wise and the mixture was stirred for 1 h at −78° C. The reaction was quenched with aqueous ammonium chloride and the aqueous layer was extracted twice with diethyl ether. The combined organic phase was washed with brine dried (sodium sulfate), filtered and evaporated to give 2.2 g of crude material. Precipitation in heptane and diethyl ether gave 547 mg of 9-(3,4-dichloro-phenyl)-9-hydroxy-3-aza-spiro[5.5]undecane-3-carboxylic acid tert-butyl ester. LC-ESI-HRMS of [M+H]+ shows 296.0983 Da. Calc. 296.09728 Da, dev. 3.4 ppm.

후처리

  1. stirringthe mixture was stirred for 1 h at −78° C
  2. customThe reaction was quenched with aqueous ammonium chloride
  3. extractionthe aqueous layer was extracted twice with diethyl ether
  4. washThe combined organic phase was washed with brine
  5. dry with materialdried (sodium sulfate)
  6. filtrationfiltered
  7. customevaporated
  8. customto give 2.2 g of crude material
  9. customPrecipitation in heptane

출처 및 근거

ORD 기록
ord-a109325ed10945438551e83f508937fc
출처 데이터셋
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08093388B2

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