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1,2-Dichloroethane → N-[1-(5-Ethyl-[1,3,4]oxadiazole-2-carbonyl)-butyl]-4-oxo-2-benzylsulfonyl-methyl-4-pyrrolidin-1-yl-butyramide

HRID 1830174
ノート
印刷プレビュー

反応式

HRID 1830174 の反応式
C1(C(=O)C[CH:8]([CH2:12][S:13]([CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)(=[O:15])=[O:14])[C:9]([OH:11])=O)CCCC1.Cl.[NH2:25][CH:26]([CH2:36][CH2:37][CH3:38])[CH:27]([C:29]1[O:30][C:31]([CH2:34][CH3:35])=[N:32][N:33]=1)[OH:28].[CH:39]1[CH:40]=CC2N(O)N=[N:45][C:43]=2[CH:44]=1.C(Cl)CCl.CN1CC[O:57][CH2:56]C1.[CH3:60]C(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.[O-]S([O-])(=S)=O.[Na+].[Na+].C([O-])(O)=O.[Na+]>C(Cl)Cl>[CH2:34]([C:31]1[O:30][C:29]([C:27]([CH:26]([NH:25][C:56](=[O:57])[C:12]([CH3:60])([S:13]([CH2:16][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)(=[O:14])=[O:15])[CH2:8][C:9](=[O:11])[N:45]2[CH2:40][CH2:39][CH2:44][CH2:43]2)[CH2:36][CH2:37][CH3:38])=[O:28])=[N:33][N:32]=1)[CH3:35]
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 7

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 757711-HydroxybenzotriazoleHCID 159087TriacetoxyperiodinaneHCID 220540264-Cyclopentyl-4-oxo-2-benzylsulfonylmethyl-butyric acidHCID 22607107sodium thiosulfate NaHCO3
HCID 69434054
2-amino-1-(5-ethyl-1,3,4-oxadiazole-2-yl)-1-pentanol HCl salt

生成物 1

HCID 22054102N-[1-(5-Ethyl-[1,3,4]oxadiazole-2-carbonyl)-butyl]-4-oxo-2-benzylsulfonyl-methyl-4-pyrrolidin-1-yl-butyramide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred mixture 4-cyclopentyl-4-oxo-2-benzylsulfonylmethyl-butyric acid (169.5 mg, 0.5 mmol), 2-amino-1-(5-ethyl-1,3,4-oxadiazole-2-yl)-1-pentanol HCl salt (117.5 mg), and HOBt (91.8 mg, 0.6 mmol) in MeCl2 5 ml), was added EDC (144 mg, 0.75 mmol) and N-methylmorpholine (0.3 ml) at room temperature. After stirring for 14 hours, the reaction mixture was extracted with ethyl acetate. The organic layer was washed with saturated NaHCO3, brine, dried with MgSO4 and concentrated to yield 240 mg of crude product. The crude product was treated with Dess-Martin periodinane (343 mg, 0.693 mmol) at room temperature in 5 mls of MeCl2. After stirring for 1 hour, 5 mls of saturated Na2S2O3—NaHCO3 were added. After a further 0.5 hours, the reaction mixture was extracted with ethyl acetate, washed with brine, dried with MgSO4 and concentrated. The residue was purified with silica gel column chromatography to yield 145 mg of N-[1-(5-Ethyl-[1,3,4]oxadiazole-2-carbonyl)-butyl]-4-oxo-2-benzylsulfonyl-methyl-4-pyrrolidin-1-yl-butyramide; H1NMR(DMSO-d): 8.85 (½H, d, NH, diastereomeric), 8.78 (½H, d, NH, diastereomeric), 7.5–7.3(5H, m), 5.1–4.95(1H, m), 4.5–4.3 (2H, m), 3.5–3.2 (8H, m), 3.2–3(1H, m), 2.82(2H, m), 2–1.8(6H, m), 1.6–1.3(2H, m), 1.24(3H, m), 0.9–0.8(3H, m); MS: 518.2(M−1), 519.7 (M+1).

後処理

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with saturated NaHCO3, brine
  3. dry with materialdried with MgSO4
  4. concentrationconcentrated
  5. customto yield 240 mg of crude product
  6. stirringAfter stirring for 1 hour
  7. waitAfter a further 0.5 hours
  8. extractionthe reaction mixture was extracted with ethyl acetate
  9. washwashed with brine
  10. dry with materialdried with MgSO4
  11. concentrationconcentrated
  12. customThe residue was purified with silica gel column chromatography

出典と根拠

ORDレコード
ord-147fbd732acb4e9b848a1f5ee167daf3
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07064123B1

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート