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Hydrochloric Acid → methyl 4-methyl-2-(N,N-bis(methylsulphonyl)amino]benzoate

HRID 1953127
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HRID 1953127 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[NH2:6][C:7]1[CH:16]=[C:15]([CH3:17])[CH:14]=[CH:13][C:8]=1[C:9]([O:11][CH3:12])=[O:10].C(N(CC)CC)C.Cl>ClCCl>[CH3:17][C:15]1[CH:14]=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[C:7]([N:6]([S:2]([CH3:1])(=[O:4])=[O:3])[S:2]([CH3:1])(=[O:4])=[O:3])[CH:16]=1.[CH3:17][C:15]1[CH:14]=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[C:7]([NH:6][S:2]([CH3:1])(=[O:4])=[O:3])[CH:16]=1
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 11205965Methyl 2-amino-4-methylbenzoate

생성물 2

HCID 22620995methyl 4-methyl-2-(N,N-bis(methylsulphonyl)amino]benzoateHCID 22621226HCID 22621226, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Methanesulphonyl chloride (12.2 ml) was added to a stirred, cooled solution of methyl 2-amino-4-methylbenzoate (10.3 g) and triethylamine (19.5 ml) in dichloromethane while maintaining the temperature below 0° C. The mixture was stirred at room temperature for 4 hours. Hydrochloric acid solution (2M) was added and the layers were separated. The organic layer was washed with water, dried (magnesium sulphate) and filtered. The filtrate was evaporated to dryness to give a mixure of methyl 4-methyl-2-[N,N-bis(methylsulphonyl)amino]benzoate and methyl 4-methyl-2-(N-methylsulphonylamino)benzoate (18.26 g) as a yellow solid which was not further purified.

후처리

  1. temperaturewhile maintaining the temperature below 0° C
  2. customthe layers were separated
  3. washThe organic layer was washed with water
  4. dry with materialdried (magnesium sulphate)
  5. filtrationfiltered
  6. customThe filtrate was evaporated to dryness

출처 및 근거

ORD 기록
ord-a48fa280c97a47a296acb5adbc294bfc
출처 데이터셋
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06114538

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