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Cyclohexylamine → [3-(4-Cyclohexylcarbamoyl-piperidin-1-ylmethyl)-phenyl]-carbamic acid tert-butyl ester

HRID 1486691
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HRID 1486691 반응식
[C:1]([O:5][C:6]([NH:8][C:9]1[CH:10]=[C:11]([CH:22]=[CH:23][CH:24]=1)[CH2:12][N:13]1[CH2:18][CH2:17][CH:16]([C:19]([OH:21])=O)[CH2:15][CH2:14]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(Cl)(=O)C(Cl)=O.CCN(C(C)C)C(C)C.[CH:40]1([NH2:46])[CH2:45][CH2:44][CH2:43][CH2:42][CH2:41]1>C(Cl)Cl.CN(C=O)C>[C:1]([O:5][C:6](=[O:7])[NH:8][C:9]1[CH:24]=[CH:23][CH:22]=[C:11]([CH2:12][N:13]2[CH2:14][CH2:15][CH:16]([C:19](=[O:21])[NH:46][CH:40]3[CH2:45][CH2:44][CH2:43][CH2:42][CH2:41]3)[CH2:17][CH2:18]2)[CH:10]=1)([CH3:4])([CH3:2])[CH3:3]
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참가 물질

7

반응물 4

HCID 7965CyclohexylamineHCID 65578Oxalyl chlorideHCID 81531DiisopropylethylamineHCID 867065221-(3-tert-Butoxycarbonylamino-benzyl)-piperidine-4-carboxylic acid

생성물 1

HCID 86706523[3-(4-Cyclohexylcarbamoyl-piperidin-1-ylmethyl)-phenyl]-carbamic acid tert-butyl ester수율 29.4%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 6344Dichloromethane용매2회

실험 절차

A suspension of crude 1-(3-tert-butoxycarbonylamino-benzyl)-piperidine-4-carboxylic acid (6.7 g, 20 mmol) in DCM (250 mL) and DMF (0.2 mL) is treated with oxalyl chloride (25 mmol, 2.21 mL) dropwise at 0° C. during 20 min. under nitrogen. The reaction mixture is stirred at RT for 2 h. Then the solvent is evaporated under reduced pressure and dried under high vacuum. The crude acid chloride is dissolved in DCM (250 mL) and treated with DIPEA (20 mmol, 3.42 mL) and cooled down to 0° C. A solution of cyclohexylamine (2.18 g, 22 mmol) in DCM (20 mL) is added dropwise over 15 min. and the resulting mixture is stirred for 2 h. at RT. The reaction mixture is washed twice with aq. sat. NaHCO3 (100 mL) and dried over MgSO4. After evaporation of the solvent, the crude residue is purified by flash chromatography on silica gel using a mixture of DCM/MeOH 9:1. After concentration of the product containing fractions, the title compound (2.44 g, 29%) is obtained as a beige powder: LC-MS A: tR=0.66 min; [M+H]+=416.2.

후처리

  1. customThen the solvent is evaporated under reduced pressure
  2. customdried under high vacuum
  3. dissolutionThe crude acid chloride is dissolved in DCM (250 mL)
  4. temperaturecooled down to 0° C
  5. stirringthe resulting mixture is stirred for 2 h. at RT
  6. washThe reaction mixture is washed twice with aq. sat. NaHCO3 (100 mL)
  7. dry with materialdried over MgSO4
  8. customAfter evaporation of the solvent
  9. customthe crude residue is purified by flash chromatography on silica gel using
  10. additiona mixture of DCM/MeOH 9:1
  11. additionAfter concentration of the product containing fractions

출처 및 근거

ORD 기록
ord-224fd679768749c6b68316bb8170ca4d
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09428456B2

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