Acetonitrile → Tert-butyl 3-hydrazinylpropanoate

HRID 582686

反応式

HRID 582686 の反応式
Cl.[NH2:2][CH2:3][C@H:4](NS(C1C=CC=CC=1)(=O)=O)[C:5]([O:7][C:8]([CH3:11])([CH3:10])[CH3:9])=[O:6].F[P-](F)(F)(F)(F)F.[N:29]1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.CN1CCOCC1.CC#N>C(OCC)(=O)C>[C:8]([O:7][C:5](=[O:6])[CH2:4][CH2:3][NH:2][NH2:29])([CH3:11])([CH3:10])[CH3:9]

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 79724-MethylmorpholineHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 22853534(S)-3-amino-2-benzenesulfonylamino-propionic acid tert-butyl ester hydrochloride

生成物 1

HCID 11040997Tert-butyl 3-hydrazinylpropanoate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A solution of acid 2-7 (380 mg, 1.19 mmole), amine 1-4 (362 mg, 1.19 mmole), BOP (789 mg, 1.79 mmole), NMM (521 μl, 4.76 mmole) and CH3CN (6 ml) was stirred at ambient temperature for 20 h. The reaction was diluted with ethyl acetate and then washed with H2O, sat. NaHCO3, 10% KHSO4, brine, dried (MgSO4) and concentrated. Flash chromotography (silica, EtOAc) gave the ester 2-8 as a white solid.

後処理

  1. washwashed with H2O, sat. NaHCO3, 10% KHSO4, brine
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-377dd23692be4b98a357a7e8ec328630
出典データセット
uspto-grants-1999_07
特許番号
US05925655

関連ノート

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