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Lithium Chloride → Tert-butyl 2-(3-(3-chloro-4-(2-hydroxyethyl)phenyl)ureido)cyclohexylcarbamate

HRID 1023860
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HRID 1023860 반응식
[C:1]([O:5][C:6]([NH:8][CH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH:10]1[NH:15][C:16](=[O:31])[NH:17][C:18]1[CH:23]=[CH:22][C:21]([CH2:24][C:25](OCC)=[O:26])=[C:20]([Cl:30])[CH:19]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[BH4-].[Na+].[Li+].[Cl-]>C1COCC1.CCO>[Cl:30][C:20]1[CH:19]=[C:18]([NH:17][C:16](=[O:31])[NH:15][CH:10]2[CH2:11][CH2:12][CH2:13][CH2:14][CH:9]2[NH:8][C:6](=[O:7])[O:5][C:1]([CH3:2])([CH3:3])[CH3:4])[CH:23]=[CH:22][C:21]=1[CH2:24][CH2:25][OH:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 433294Lithium ChlorideHCID 4311764Sodium borohydrideHCID 67204990Ethyl 2-(4-(3-(2-(tert-butoxycarbonylamino)cyclohexyl)ureido)-2-chlorophenyl)acetate

생성물 1

HCID 67206716Tert-butyl 2-(3-(3-chloro-4-(2-hydroxyethyl)phenyl)ureido)cyclohexylcarbamate

시약·촉매·용매 1

HCID 21873804Tetrahydrofuran ethanol용매

실험 절차

To a solution of ethyl 2-(4-(3-(2-(tert-butoxycarbonylamino)cyclohexyl)ureido)-2-chlorophenyl)acetate (452 mg, 0.996 mmol) in a mixture of THF:EtOH (1:2, 12 mL) at room temperature, was added NaBH4 (124 mg, 3.29 mmol) and LiCl (139 mg, 3.29 mmol). The reaction mixture was stirred overnite. The solvents were distilled off and the crude was diluted with saturated aqueous NH4Cl (20 mL), the product was extracted with ethyl acetate (2×20 mL). The combined organic extracts were dried over Na2SO4 and the solvent distilled off under reduced pressure. The crude product was purified by flash column chromatography to separate cis 964 mg, 0.155 mmol) and trans (83 mg, 0.201 mmol) diastereomers. These alcohols were converted into tosylates using general procedure for the preparation of tosylates. 1H NMR (cis): 1.23-1.26 (m, 3H), 1.36 (s, 9H), 1.70-1.74 (m, 2H), 1.99-2.06 (m, 2H), 2.41-2.43 (m, 1H), 2.92 (t, 2H, J=6.4 Hz), 3.25-3.29 (m, 1H), 3.51-3.54 (m, 1H), 3.83-3.86 (m, 2H), 5.03 (d, 1H, J=8.8 Hz), 5.62 (d, 1H, J=8.4 Hz), 7.04 (d, 1H, J=8.4 Hz), 7.09 (d, 1H, J=8 Hz), 7.32 (s, 2H). 1H NMR (trans): 1.26-1.29 (m, 1H), 1.37-1.42 (m, 12H), 1.69-1.72 (m, 2H), 1.97 (s, 1H), 2.53-2.55 (m, 1H), 2.85 (t, 2H, J=6.4 Hz), 3.75-3.77 (m, 3H), 3.97-3.99 (m, 1H), 5.15 (br s, 1H), 5.86 (br s, 1H), 6.98-7.05 (m, 2H), 7.30 (s, 1H), 7.41 (s, 2H).

후처리

  1. distillationThe solvents were distilled off
  2. additionthe crude was diluted with saturated aqueous NH4Cl (20 mL)
  3. extractionthe product was extracted with ethyl acetate (2×20 mL)
  4. dry with materialThe combined organic extracts were dried over Na2SO4
  5. distillationthe solvent distilled off under reduced pressure
  6. customThe crude product was purified by flash column chromatography
  7. customto separate cis 964 mg, 0.155 mmol) and trans (83 mg, 0.201 mmol) diastereomers
  8. customThese alcohols were converted into tosylates using general procedure for the preparation of tosylates

출처 및 근거

ORD 기록
ord-2cf8acc454574a6f8fa4b384e0ae93bf
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08722720B2

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