4-Methylmorpholine → Ethyl acetate ethanol ammonia

HRID 322498ノート

反応式

HRID 322498 の反応式
[O:1]=[C:2]1[CH:7](CCC2C=CC3CCCNC=3N=2)CCC[N:3]1[CH2:20][C:21]([OH:23])=[O:22].CN1CCO[CH2:27][CH2:26]1.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1>CC#N>[NH3:3].[CH3:7][CH2:2][OH:1].[CH3:26][CH2:27][O:23][C:21]([CH3:20])=[O:22]

参加物

5

反応物 3

HCID 79724-MethylmorpholineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 22008800HCID 22008800、化合物

生成物 1

HCID 86587043Ethyl acetate ethanol ammonia

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A stirred mixture of 1-8 (71 mg, 0.20 mmol), 1-9 (59 mg, 0.22 mmol) (Rico et al., J. Org. Chem., 1993, 58, 7948), NMM (88 μL, 0.8 mmol), and CH3CN (25 mL) was treated with BOP (97 mg, 0.22 mmol). After 24 h, the reaction mixture was concentrated to dryness, dissolved in EtOAc, and then washed with H2O, dried (MgSO4), and concentrated. Flash chromatography (silica, 10% (NH3/EtOH/EtOAc) gave 1-10 as a colorless gum.

後処理

  1. concentrationthe reaction mixture was concentrated to dryness
  2. dissolutiondissolved in EtOAc
  3. washwashed with H2O
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-6ed823079f2249778c51d799d559c2c1
出典データセット
uspto-grants-2001_04
特許番号
US06211184B1

反応ノート

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