Acetonitrile → Tert-butyl 3-hydrazinylpropanoate

HRID 582686

반응식

HRID 582686 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

HCID 11040997Tert-butyl 3-hydrazinylpropanoate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-377dd23692be4b98a357a7e8ec328630
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925655

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