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1,2-Dichloroethane → Morpholine-4-carboxylic acid [1-(2-benzylcarbamoyl-2-oxo-ethylcarbamoyl)-2-phenylmethanesulfonyl-ethyl]-amide

HRID 460416
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HRID 460416 반응식
C(O[C:6](=[O:21])[NH:7][CH2:8][CH:9]([C:11](=[O:20])[NH:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[OH:10])(C)(C)C.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.[N:36]1([C:42]([NH:44][CH:45]([CH2:49][S:50]([CH2:53][C:54]2[CH:59]=[CH:58][CH:57]=[CH:56][CH:55]=2)(=[O:52])=[O:51])C(O)=O)=[O:43])[CH2:41][CH2:40][O:39][CH2:38][CH2:37]1.CN1CCOCC1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>ClCCl.FC(F)(F)C(O)=O>[CH2:13]([NH:12][C:11]([C:9](=[O:10])[CH2:8][NH:7][C:6]([CH:45]([NH:44][C:42]([N:36]1[CH2:41][CH2:40][O:39][CH2:38][CH2:37]1)=[O:43])[CH2:49][S:50]([CH2:53][C:54]1[CH:55]=[CH:56][CH:57]=[CH:58][CH:59]=1)(=[O:52])=[O:51])=[O:21])=[O:20])[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1
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참가 물질

9

반응물 6

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 159087TriacetoxyperiodinaneHCID 112797342-[(Morpholine-4-carbonyl)-amino]-3-phenylmethanesulfonyl-propionic acidHCID 69445033(2-Benzylcarbamoyl-2-hydroxy-ethyl)-carbamic acid tert-butyl ester

생성물 1

HCID 10186753Morpholine-4-carboxylic acid [1-(2-benzylcarbamoyl-2-oxo-ethylcarbamoyl)-2-phenylmethanesulfonyl-ethyl]-amide수율 51.8%

시약·촉매·용매 2

HCID 6344Dichloromethane용매2회HCID 6422Trifluoroacetic acid용매

실험 절차

(2-Benzylcarbamoyl-2-hydroxy-ethyl)-carbamic acid tert-butyl ester (0.2 g, 0.68 mmol) was dissolved in dichloromethane (2 mL) and trifluoroacetic acid (2 mL). After stirring for 2 h at ambient temperature, the solution was evaporated under vacuum and the residue was dried under high vacuum. To this residue were added EDC (200 mg, 1.05 mmol), HOBt (200 mg, 1.28 mmol), 2-[(Morpholine-4-carbonyl)-amino]-3-phenylmethanesulfonyl-propionic acid (200 mg, 0.56 mmol), dichloromethane (5 mL) and 4-methylmorpholine (0.5 mL). The mixture was stirred at ambient temperature for 2 h. After dilution with ethyl acetate (100 mL) the solution was washed with 1N aqu. HCl (30 mL), sat. aqu. NaHCO3 (30 mL) and brine (30 mL), dried with MgSO4 and evaporated under vacuum. The crude product was dissolved in dichloromethane (10 mL). Dess-Martin periodinane (500 mg, 1.18 mmol) was added, and the reaction mixture was stirred at ambient temperature for 1 h. After dilution with ethyl acetate (100 mL), the solution was washed with 0.26M Na2S2O3 in sat. aqu. NaHCO3 (30 mL), sat. aqu. NaHCO3 and brine, dried with MgSO4, and evaporated under vacuum. The product (morpholine-4-carboxylic acid [1-(2-benzylcarbamoyl-2-oxo-ethylcarbamoyl)-2-phenylmethanesulfonyl-ethyl]-amide) was crystallized from ethyl acetate/diethylether and was obtained as a white solid (153 mg, 0.29 mmol). 1H NMR: (DMSO) 9.24 (t, J=6.4 Hz, 1H), 8.19 (t, J=5.6 Hz, 1H), 7.39–7.19 (m, 10H), 7.08 (d, J=8 Hz, 1H), 4.83–4.76 (m, 1H), 4.49 (s, 2H), 4.48–4.33 (m, 2H), 4.31 (d, J=6.8 Hz, 2H), 3.68–3.25 (m, 10H). MS: (M+H)+ 531.

후처리

  1. customthe solution was evaporated under vacuum
  2. customthe residue was dried under high vacuum
  3. stirringThe mixture was stirred at ambient temperature for 2 h
  4. washAfter dilution with ethyl acetate (100 mL) the solution was washed with 1N aqu
  5. dry with materialNaHCO3 (30 mL) and brine (30 mL), dried with MgSO4
  6. customevaporated under vacuum
  7. dissolutionThe crude product was dissolved in dichloromethane (10 mL)
  8. stirringthe reaction mixture was stirred at ambient temperature for 1 h
  9. washAfter dilution with ethyl acetate (100 mL), the solution was washed with 0.26M Na2S2O3 in sat. aqu
  10. dry with materialNaHCO3 and brine, dried with MgSO4
  11. customevaporated under vacuum
  12. customThe product (morpholine-4-carboxylic acid [1-(2-benzylcarbamoyl-2-oxo-ethylcarbamoyl)-2-phenylmethanesulfonyl-ethyl]-amide) was crystallized from ethyl acetate/diethylether

출처 및 근거

ORD 기록
ord-50ef4d1db5a24eadaab8d9bef1530816
출처 데이터셋
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07196099B2

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