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3-Chloroaniline → HCID 86700762, 화합물

HRID 2174419
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HRID 2174419 반응식
Br[C:2]1[N:7]=[CH:6][C:5]([C@@H:8]2[CH2:10][C@H:9]2[NH:11][C:12](=[O:18])[O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:4][CH:3]=1.[Cl:19][C:20]1[CH:21]=[C:22]([CH:24]=[CH:25][CH:26]=1)[NH2:23].CC(C)([O-])C.[Na+]>O1CCOCC1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:19][C:20]1[CH:21]=[C:22]([NH:23][C:2]2[N:7]=[CH:6][C:5]([C@@H:8]3[CH2:10][C@H:9]3[NH:11][C:12](=[O:18])[O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[CH:4][CH:3]=2)[CH:24]=[CH:25][CH:26]=1
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참가 물질

6

반응물 3

HCID 79323-ChloroanilineHCID 23676156Sodium t-butoxideHCID 86691195rac-tert-butyl N-((1R,2S)-2-(6-bromopyridin-3-yl)cyclopropyl)carbamate2회

생성물 1

HCID 86700762HCID 86700762, 화합물수율 63%

시약·촉매·용매 2

HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 31275
1,4-Dioxane
용매

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온도
80 °C

실험 절차

A solution of tert-butyl (trans)-2-(6-bromopyridin-3-yl)cyclopropylcarbamate (Intermediate E, 250 mg, 0.798 mmol), 3-chloroaniline (122 mg, 0.958 mmol), Sodium tert-butoxide (115 mg, 1.198 mmol) in 1,4-dioxane (5 mL) was degassed for 30 min, tris(dibenzylidene acetone)dipalladium(0) (36 mg, 0.039 mmol) and 4,5-Bis(diphenyl phosphino)-9,0-dimethyl xanthene (138 mg, 0.39 mmol) was added and heated for 4 h at 80° C. After completion, the solvent was evaporated; the residue was poured into ice cold water (10 mL) and extracted with EtOAc (2×20 mL). The combined extracts were washed with water (10 mL), brine (10 mL), dried over anhydrous Na2SO4, filtered and evaporated. The crude residue was purified by flash chromatography to give tert-butyl (trans)-2-(6-(3-chlorophenylamino)pyridin-3-yl)cyclopropylcarbamate (180 mg, 63%) as white solid.

후처리

  1. customAfter completion, the solvent was evaporated
  2. additionthe residue was poured into ice cold water (10 mL)
  3. extractionextracted with EtOAc (2×20 mL)
  4. washThe combined extracts were washed with water (10 mL), brine (10 mL)
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationfiltered
  7. customevaporated
  8. customThe crude residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-97fa78c5c0634947ae0f7a3cd1ca349e
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09061966B2

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