Hydrochloric Acid → Methyl 2-amino-4-{[(methylsulfonyl)amino]methyl}benzoate

HRID 1862596노트

반응식

HRID 1862596 반응식
[CH3:1][S:2]([NH:5][CH2:6][C:7]1[CH:16]=[CH:15][C:10]([C:11]([O:13][CH3:14])=[O:12])=[C:9]([N+:17]([O-])=O)[CH:8]=1)(=[O:4])=[O:3].Cl.[H][H]>CO.[Pd]>[NH2:17][C:9]1[CH:8]=[C:7]([CH2:6][NH:5][S:2]([CH3:1])(=[O:4])=[O:3])[CH:16]=[CH:15][C:10]=1[C:11]([O:13][CH3:14])=[O:12]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 22494948HCID 22494948, 화합물HCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 11288376Methyl 2-amino-4-{[(methylsulfonyl)amino]methyl}benzoate수율 88%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

13.25 g (46 mmol) of methyl 4-methanesulfonylaminomethyl-2-nitrobenzoate are dissolved in 200 ml of methanol. After addition of 1.4 ml (46 mmol) of concentrated hydrochloric acid and 1 g of Pd catalyst (10% on active charcoal), the mixture is hydrogenated with hydrogen under atmospheric pressure until the hydrogen uptake is complete. The mixture is removed from the catalyst by filtration and the filtrate is concentrated completely. Crystallization of the residue from water yields 10.4 g (88%) of methyl 2-amino-4-methanesulfonylaminomethylbenzoate of melting point 121-122° C.

후처리

  1. customThe mixture is removed from the catalyst by filtration
  2. concentrationthe filtrate is concentrated completely
  3. customCrystallization of the residue from water

출처 및 근거

ORD 기록
ord-3589798437004ad794164a3b8670f7d4
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06538150B2

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