Water → Methyl 4-(3-chloro-propyl-sulphonyl-amino)-3-methyl-benzoate

HRID 1629839노트

반응식

HRID 1629839 반응식
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[CH3:12].[Cl:13][CH2:14][CH2:15][CH2:16][S:17](Cl)(=[O:19])=[O:18].O.C(OCC)(=O)C>N1C=CC=CC=1>[Cl:13][CH2:14][CH2:15][CH2:16][S:17]([NH:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[CH3:12])(=[O:19])=[O:18]

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 154103-Chloropropanesulphonyl chlorideHCID 2736799Methyl 4-amino-3-methylbenzoate

생성물 1

HCID 43654282Methyl 4-(3-chloro-propyl-sulphonyl-amino)-3-methyl-benzoate

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

100 mg (0.61 mmol) methyl 4-amino-3-methyl-benzoate dissolved in 3 ml of pyridine are combined with 82 μl (0.67 mmol) 3-chloropropanesulphonic acid chloride and stirred for 16 hours at ambient temperature. The reaction solution is combined with water and ethyl acetate and then the aqueous phase is again extracted with ethyl acetate. The combined organic phases are dried over sodium sulphate and evaporated down i. vac. The residue is further reacted without any more purification.

후처리

  1. extractionthe aqueous phase is again extracted with ethyl acetate
  2. dry with materialThe combined organic phases are dried over sodium sulphate
  3. customevaporated down i
  4. customThe residue is further reacted without any more purification

출처 및 근거

ORD 기록
ord-28acd9d26007416288f95e8329d8ad61
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08791103B2

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