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

HRID 460416
ノート
印刷プレビュー

反応式

HRID 460416 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 6422Trifluoroacetic acid溶媒

実験手順

(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.

後処理

  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

出典と根拠

ORDレコード
ord-50ef4d1db5a24eadaab8d9bef1530816
出典データセット
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07196099B2

反応ノート

読み込み中…

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