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Triethylamine → 7-((4-(2,6-Dichlorophenyl)-1-piperidinyl)carbonyl)-6,7,8,9-tetrahydro-1-methyl-5H-benzocyclohepten-5-one

HRID 1241882
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HRID 1241882 반응식
[CH3:1][C:2]1[C:7]2[CH2:8][CH2:9][CH:10]([C:14]([OH:16])=O)[CH2:11][C:12](=[O:13])[C:6]=2[CH:5]=[CH:4][CH:3]=1.C(Cl)(=O)C(Cl)=O.Cl.[Cl:24][C:25]1[CH:30]=[CH:29][CH:28]=[C:27]([Cl:31])[C:26]=1[CH:32]1[CH2:37][CH2:36][NH:35][CH2:34][CH2:33]1.C(N(CC)CC)C>C(Cl)Cl.O>[CH3:1][C:2]1[C:7]2[CH2:8][CH2:9][CH:10]([C:14]([N:35]3[CH2:34][CH2:33][CH:32]([C:26]4[C:25]([Cl:24])=[CH:30][CH:29]=[CH:28][C:27]=4[Cl:31])[CH2:37][CH2:36]3)=[O:16])[CH2:11][C:12](=[O:13])[C:6]=2[CH:5]=[CH:4][CH:3]=1
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참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 11229708HCID 11229708, 화합물HCID 219369304-(2,6-dichloro-phenyl)-piperidine hydrochloride

생성물 1

HCID 219369597-((4-(2,6-Dichlorophenyl)-1-piperidinyl)carbonyl)-6,7,8,9-tetrahydro-1-methyl-5H-benzocyclohepten-5-one수율 71%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6344Dichloromethane용매2회

실험 절차

1 g (4.58 mmol) of (±)-1-methyl-5-oxo-6,7,8,9-tetrahydro-5H-benzocycloheptene-7-carboxylic acid was dissolved in 40 mL of dry CH2Cl2 and 1.2 mL (13.74 mmol) of oxalyl chloride were added dropwise at 0° C. under a nitrogen atmosphere. The solution was allowed to warm to room temperature overnight, then the solvent and the excess oxalyl chloride were removed in vacuo. The resulting acyl chloride was dissolved in 20 mL of dry CH2Cl2 and added to a solution of 1.22 g (4.58 mmol) of 4-(2,6-dichloro-phenyl)-piperidine hydrochloride and 1.91 mL (13.74 mmol) of triethylamine in 30 mL of dry CH2Cl2 at 0° C. The reaction mire was allowed to warm to room temperature overnight, water was added, the organic phase was collected, washed with 1 N HCl solution and dried. The solvent was removed in vacuo and the resulting crude product was purified by flash chromatography, eluting with a mixture Et2O/Hexane 8:2 respectively, yielding 1.4 g of the title compound.

후처리

  1. customthe solvent and the excess oxalyl chloride were removed in vacuo
  2. dissolutionThe resulting acyl chloride was dissolved in 20 mL of dry CH2Cl2
  3. temperatureto warm to room temperature overnight
  4. customthe organic phase was collected
  5. washwashed with 1 N HCl solution
  6. customdried
  7. customThe solvent was removed in vacuo
  8. customthe resulting crude product was purified by flash chromatography
  9. washeluting with a mixture Et2O/Hexane 8:2 respectively

출처 및 근거

ORD 기록
ord-cffcfb8c3f224bb2bf84760cc556b93d
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07115633B2

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