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4-Methylmorpholine → 1-Boc-4-(2-(4-Fluoro-3-(trifluoromethyl)phenyl)-2-oxoethylcarbamoyl)piperidine

HRID 2283945
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HRID 2283945 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([C:14]([OH:16])=O)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CN1CCOCC1.CC(C)CC(Cl)=O.[Cl-].[F:32][C:33]1[CH:38]=[CH:37][C:36]([C:39](=[O:42])[CH2:40][NH3+:41])=[CH:35][C:34]=1[C:43]([F:46])([F:45])[F:44]>C1COCC1>[F:32][C:33]1[CH:38]=[CH:37][C:36]([C:39](=[O:42])[CH2:40][NH:41][C:14]([CH:11]2[CH2:10][CH2:9][N:8]([C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])[CH2:13][CH2:12]2)=[O:16])=[CH:35][C:34]=1[C:43]([F:44])([F:45])[F:46]
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참가 물질

6

반응물 4

HCID 79724-MethylmorpholineHCID 66054Isovaleryl chlorideHCID 3928711-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acidHCID 89442701[2-[4-Fluoro-3-(trifluoromethyl)phenyl]-2-oxoethyl]azanium;chloride

생성물 1

HCID 534391291-Boc-4-(2-(4-Fluoro-3-(trifluoromethyl)phenyl)-2-oxoethylcarbamoyl)piperidine수율 71.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-10 °C

실험 절차

To a solution of piperidine-1,4-dicarboxylic acid mono-tert-butyl ester (9611.92 mg; 41.92 mmol; 1.08 eq.) in THF 100 ml, added 4-methyl-morpholine (14.51 ml; 131.98 mmol; 3.40 eq.), The reaction mixture was cooled to −10° C., 3-methyl-butyryl chloride (5.03 ml; 38.82 mmol; 1.00 eq.) was add dropwise and maintaining the temperature below −5° C. after stirring for 30 mins at from −5° C. to 10° C., 2-(4-Fluoro-3-trifluoromethyl-phenyl)-2-oxo-ethyl-ammonium chloride (10.00 g; 38.82 mmol; 1.00 eq.) was added at −5° C. and stirred the mixture for 20 mins and then RT for 1 h. Added brine, extracted with EA, washed with brine, dried and concentrated. The crude oil was treated with ether. The white solid was collected as the title compound (12 g, yield 71.5%).

후처리

  1. temperaturemaintaining the temperature below −5° C.
  2. additionwas added at −5° C.
  3. waitRT for 1 h
  4. extractionAdded brine, extracted with EA
  5. washwashed with brine
  6. customdried
  7. concentrationconcentrated
  8. additionThe crude oil was treated with ether

출처 및 근거

ORD 기록
ord-ca0a5c2d2eae40bfb4f34a7e278f05b6
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09145392B2

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