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Methyl 2-[(tert-butylamino)sulfonyl]-6-nitrobenzoate → HCID 22024119, 화합물

HRID 1792891
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HRID 1792891 반응식
[C:1]([NH:5][S:6]([C:9]1[CH:18]=[CH:17][CH:16]=[C:15]([N+:19]([O-])=O)[C:10]=1[C:11]([O:13][CH3:14])=[O:12])(=[O:8])=[O:7])([CH3:4])([CH3:3])[CH3:2]>[Pd]>[NH2:19][C:15]1[CH:16]=[CH:17][CH:18]=[C:9]([S:6]([NH:5][C:1]([CH3:4])([CH3:3])[CH3:2])(=[O:8])=[O:7])[C:10]=1[C:11]([O:13][CH3:14])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 22024122Methyl 2-[(tert-butylamino)sulfonyl]-6-nitrobenzoate

생성물 1

HCID 22024119HCID 22024119, 화합물수율 86%

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

A solution of 8.00 g (25.3 mmol) of methyl 2-[(tert-butylamino)sulfonyl]-6-nitrobenzoate is admixed with 3.2 g of palladium on activated carbon (5%) and hydrogenated at room temperature and under atmospheric pressure for 6 h. The reaction mixture is then filtered, the filtrate is concentrated to dryness and the residue is purified by silica gel chromatography [TLC (SiO2)ethyl acetate/n-heptane 1:1; Rf=0.38] using ethyl acetate/n-heptane (1:1). Evaporation gives 6.23 g (86% of theory) of methyl 2-amino-6-[(tert-butylamino)sulfonyl]benzoate as a beige solid of melting point 132-133° C.

후처리

filtration
The reaction mixture is then filtered
  • concentrationthe filtrate is concentrated to dryness
  • customthe residue is purified by silica gel chromatography [TLC (SiO2)ethyl acetate/n-heptane 1:1; Rf=0.38]
  • customEvaporation
  • 출처 및 근거

    ORD 기록
    ord-e109df869bcb46d5a4484519939d7541
    출처 데이터셋
    uspto-grants-2006_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US07078369B2

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