4-Methylmorpholine → 4-(Methyloxycarbonyl)benzoyl-2(S)-phenylsulfonylamino-beta-alanine t-butyl ester

HRID 265906

反応式

HRID 265906 の反応式
C[C:2]1[CH:10]=[C:9]([C:11]([OH:13])=[O:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.Cl.[C:15]1([S:21]([NH:24][C@@H:25]([CH2:33][NH2:34])[C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])(=[O:23])=[O:22])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[CH3:35]N1CCOCC1.CN([P+](ON1N=NC2C=CC=CC1=2)(N(C)C)N(C)C)C.F[P-](F)(F)(F)(F)F>C(#N)C.CCOC(C)=O>[C:29]([O:28][C:26](=[O:27])[C@@H:25]([NH:24][S:21]([C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)(=[O:22])=[O:23])[CH2:33][NH:34][C:4](=[O:6])[C:3]1[CH:2]=[CH:10][C:9]([C:11]([O:13][CH3:35])=[O:12])=[CH:8][CH:7]=1)([CH3:30])([CH3:31])[CH3:32]

参加物

7

反応物 4

HCID 79724-MethylmorpholineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 2280862-Methylterephthalic acidHCID 22853534(S)-3-amino-2-benzenesulfonylamino-propionic acid tert-butyl ester hydrochloride

生成物 1

HCID 867510984-(Methyloxycarbonyl)benzoyl-2(S)-phenylsulfonylamino-beta-alanine t-butyl ester

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A slurry of mono-methyl terephthalic acid (32-1, Aldrich) (0.25 g, 1.4 mmol) and 19-2a (0.5 g, 1.4 mmol) in acetonitrile (7 mL) was treated with N-methyl morpholine (0.31 mL, 2.8 mmol) and BOP reagent (0.62 g, 1.4 mmol) for 24 h. The solution was diluted with EtOAc, washed with H2O, 10% KHSO4, saturated NaHCO3 and brine. The organic layer was dried over MgSO4, filtered and evaporated to give a tan solid. Column chromatography (40% EtOAc/Hexanes) gave 32-2 as a white solid.

後処理

  1. washwashed with H2O, 10% KHSO4, saturated NaHCO3 and brine
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. customevaporated
  5. customto give a tan solid

出典と根拠

ORDレコード
ord-112c5f47032b47e4a4a80acb7046b6b1
出典データセット
uspto-grants-1997_07
特許番号
US05648368

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