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1,2-Dichloroethane → HCID 11754542, 화합물

HRID 225773
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HRID 225773 반응식
C(Cl)CCl.C(N(C(C)C)CC)(C)C.C(N)C1C=CC=CC=1.[CH3:22][C:23]1[CH:39]=[CH:38][C:26]([C:27]([N:29]2[CH2:34][CH2:33][CH2:32][CH2:31][CH:30]2[C:35](O)=O)=[O:28])=[CH:25][CH:24]=1.[CH2:40]([NH:47][C:48]([C:50]1[CH:55]=[CH:54][C:53]([Cl:56])=[CH:52][C:51]=1[NH-:57])=[O:49])[C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1>>[CH2:40]([N:47]1[C:48](=[O:49])[C:50]2[C:51](=[CH:52][C:53]([Cl:56])=[CH:54][CH:55]=2)[N:57]=[C:35]1[CH:30]1[CH2:31][CH2:32][CH2:33][CH2:34][N:29]1[C:27](=[O:28])[C:26]1[CH:38]=[CH:39][C:23]([CH3:22])=[CH:24][CH:25]=1)[C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 111,2-DichloroethaneHCID 7504BenzylamineHCID 81531DiisopropylethylamineHCID 167698421-(4-Methylbenzoyl)piperidine-2-carboxylic acidHCID 178514215HCID 178514215, 화합물

생성물 1

HCID 11754542HCID 11754542, 화합물수율 47%

실험 절차

Formula 205 where T is a covalent bond; W, X, Y and Z are —C═; U—V is —N(R6)—CReRf—CRgRh—; R1, R2, R4 and Ra to Rh are H; Rand R6 is p-methyl-benzoyl: A mixture of the compound of Formula 203 (2.66 g, 6.7 mmol), 1M NaOH (27 mL), methanol (54 mL), and dioxane (36 mL) was stirred at room temperature for 7 hours. The solvents were evaporated and the residue portioned between dichloromethane (75 mL), saturated NaCl (50 mL), and concentrated HCl (3 mL). The layers were separated and the organic layer dried over MgSO4 and concentrated under vacuum to give the corresponding compound of Formula 204, 4-chloro-2-[1-(4-methyl-benzoyl)-piperidine-2-carbonyl]amino}-benzoic acid, which was carried forward without further purification. This crude product was redissolved in dichloromethane and treated with EDC (3.84 g, 20 mmol), and diisopropylethylamine (3.50 mL, 20 mmol). After stirring 20 minutes, benzylamine (2.20 mL, 20 mmol) was added and the mixture stirred overnight at room temperature. The mixture was washed with water (2×50 mL) and 1M HCl, dried over MgSO4, filtered and concentrated under vacuum to give 1.5 g (47% yield) of the desired product of Formula 205, 1-(4-methyl-benzoyl)-piperidine-2-carboxylic acid (2-benzylcarbamoyl-5-chloro-phenyl-amide, a crude product that was found to be 80% pure by reverse phase HPLC. The product was taken on without further purification. LRMS (MH+) m/z 491.

후처리

  1. customwas carried forward without further purification
  2. dissolutionThis crude product was redissolved in dichloromethane
  3. stirringthe mixture stirred overnight at room temperature
  4. washThe mixture was washed with water (2×50 mL) and 1M HCl
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-879cb533180c4014998c1edc2da0fde4
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07557115B2

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