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Dichloromethane → HCID 46870768, 화합물

HRID 1400221
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HRID 1400221 반응식
[NH2:1][C:2](=[O:31])[CH:3]([OH:30])[CH:4]([NH:12][C:13]([C:15]1[C:16]([C:21]2[S:22][C:23]3[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=3[N:25]=2)=[N:17][CH:18]=[CH:19][CH:20]=1)=[O:14])[CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.ClCCl.ClC(Cl)C(O)=O>CS(C)=O>[NH2:1][C:2](=[O:31])[C:3](=[O:30])[CH:4]([NH:12][C:13]([C:15]1[C:16]([C:21]2[S:22][C:23]3[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=3[N:25]=2)=[N:17][CH:18]=[CH:19][CH:20]=1)=[O:14])[CH2:5][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 6597Dichloroacetic AcidHCID 67541222HCID 67541222, 화합물

생성물 1

HCID 46870768HCID 46870768, 화합물수율 52.1%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of N-(4-Amino-3-hydroxy-4-oxo-1-phenylbutan-2-yl)-2-(1,3-benzothiazol-2-yl)pyridine-3-carboxamide (0.5 g, 1.16 mmol) in 1.5 ml of DMSO und 15 ml of dichloromethane 3.04 g N-cyclohexylcarbodiimid-N′-methylpolystyrole (1.9 mmol/g; 5.78 mmol) and 0.24 ml dichloroacetic acid (0.38 g, 2.89 mmol) were added, and the reaction mixture stirred over night at room temperature. For work up the polymer was filtered off, washed with dichloromethane, and the combined organic layers evaporated to dryness. Treatment with a mixture of n-hexane/ethylacetate, filtration and drying afforded 260 mg of the title compound, as white amorphous solid:

후처리

  1. filtrationFor work up the polymer was filtered off
  2. washwashed with dichloromethane
  3. customthe combined organic layers evaporated to dryness
  4. additionTreatment with a mixture of n-hexane/ethylacetate, filtration
  5. customdrying

출처 및 근거

ORD 기록
ord-703661a54e9f49eda6a95f16976dbc2c
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08906941B2

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