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4-Methylmorpholine → HCID 10717338、化合物

HRID 1953051
ノート
印刷プレビュー

反応式

HRID 1953051 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([C@H:15]2[C:19](=[O:20])[NH:18][C@@H:17]([C:21]([OH:23])=O)[CH2:16]2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CN1CC[O:28][CH2:27][CH2:26]1.Cl.[CH3:32][Si:33](C)([CH3:38])[CH2:34]CON.B(F)([O-])[O-].B(F)([O-])[O-].B(F)([O-])[O-].B(F)([O-])[O-].B(F)([O-])[O-].B(F)([O-])[O-].[N:64]1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1>C(Cl)Cl>[CH3:32][Si:33]([CH3:38])([CH3:34])[CH2:26][CH2:27][O:28][NH:64][C:21]([C@H:17]1[CH2:16][C@@H:15]([C:12]2[CH:13]=[CH:14][C:9]([O:8][CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)=[CH:10][CH:11]=2)[C:19](=[O:20])[NH:18]1)=[O:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 79724-MethylmorpholineHCID 10828821HCID 10828821、化合物HCID 18419632O-(2-(Trimethylsilyl)ethyl)hydroxylamine--hydrogen chloride (1/1)HCID 86755729HCID 86755729、化合物

生成物 1

HCID 10717338HCID 10717338、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of (2R, 4S)-4-(4-benzyloxyphenyl)-5-oxo-pyrrolidine-2-carboxylic acid (330 mg, 1.06 mmol), N-methyl morpholine (0.25 mL, 2.3 mmol) and O-(2-trimethylsilylethyl) hydroxylamine hydrochloride (220 mg, 1.30 mmol) in CH2Cl2 (20 mL) was added (benztriazol-1-yloxy)tris(dimethylamino)phosphonium hexafluoroborate (560 mg, 1.27 mmol). The reaction was stirred at room temperature for 6 hours. After dilution with CH2Cl2, the mixture was washed sequentially with aqueous 0.5M HCl solution, water, aqueous saturated NaHCO3 solution, and brine. The solution was dried over MgSO4 and concentrated to a white solid that was triturated with ethyl acetate and set aside. The trituration filtrate was concentrated and chromatographed on silica gel eluting with 5% methanol in chloroform. Fractions containing the title compound were combined and concentrated to afford a white solid that was combined with the solid obtained directly from the crude product mixture. The sample was stirred in water overnight. The title compound was collected by filtration and dried. The yield was 194 mg (43%).

後処理

  1. washAfter dilution with CH2Cl2, the mixture was washed sequentially with aqueous 0.5M HCl solution, water, aqueous saturated NaHCO3 solution, and brine
  2. dry with materialThe solution was dried over MgSO4
  3. concentrationconcentrated to a white solid
  4. customthat was triturated with ethyl acetate
  5. concentrationThe trituration filtrate was concentrated
  6. customchromatographed on silica gel eluting with 5% methanol in chloroform
  7. additionFractions containing the title compound
  8. concentrationconcentrated
  9. customto afford a white solid

出典と根拠

ORDレコード
ord-9ddf5a22371345b9ad2ee675e82c375b
出典データセット
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06114361

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