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1-Hydroxybenzotriazole → 4-(2-{4-[(4-Fluorophenyl)amino]-1-piperidinyl}-2-oxoethyl)benzaldehyde

HRID 43338
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HRID 43338 반응식
[CH:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([OH:12])=O)=[CH:5][CH:4]=1)=[O:2].[F:13][C:14]1[CH:19]=[CH:18][C:17]([NH:20][CH:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)=[CH:16][CH:15]=1.Cl.CN(C)CCCN=C=NCC.ON1C2C=CC=CC=2N=N1>CN(C=O)C>[F:13][C:14]1[CH:19]=[CH:18][C:17]([NH:20][CH:21]2[CH2:26][CH2:25][N:24]([C:10](=[O:12])[CH2:9][C:6]3[CH:5]=[CH:4][C:3]([CH:1]=[O:2])=[CH:8][CH:7]=3)[CH2:23][CH2:22]2)=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 4778193N-(4-Fluorophenyl)-4-piperidinamineHCID 113441872-(4-formylphenyl)acetic Acid

생성물 1

HCID 252238954-(2-{4-[(4-Fluorophenyl)amino]-1-piperidinyl}-2-oxoethyl)benzaldehyde수율 82.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of D3 (87 mg, 0.53 mmol), D2 (102 mg, 0.53 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (123 mg, 0.64 mmol), and 1-hydroxybenzotriazole (98 mg, 0.64 mmol) in DMF (2 ml) was stirred at room temperature overnight. The DMF was removed in vacuo then EtOAc and water were added. The product was extracted into EtOAc and the combined organic layers were washed with saturated aq. NaHCO3 solution (×2) and brine then dried (Na2SO4). The solvent was removed in vacuo and the resulting residue was purified by chromatography eluting with an EtOAc/petroleum ether gradient to afford the title compound (149 mg). MS (ES): MH+ 341.

후처리

  1. customThe DMF was removed in vacuo
  2. additionEtOAc and water were added
  3. extractionThe product was extracted into EtOAc
  4. washthe combined organic layers were washed with saturated aq. NaHCO3 solution (×2) and brine
  5. dry with materialthen dried (Na2SO4)
  6. customThe solvent was removed in vacuo
  7. customthe resulting residue was purified by chromatography
  8. washeluting with an EtOAc/petroleum ether gradient

출처 및 근거

ORD 기록
ord-ec9adf3f78b34a0eb346907f339131fd
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08536182B2

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