Pyridine → HCID 54096246, 화합물

HRID 1381511노트

반응식

HRID 1381511 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]([O:11][CH3:12])=[O:10].N1C=CC=CC=1.[CH2:19]([O:21][C:22]([CH2:24][S:25](Cl)(=[O:27])=[O:26])=[O:23])[CH3:20]>C1(C)C=CC=CC=1>[CH2:19]([O:21][C:22]([CH2:24][S:25]([NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]([O:11][CH3:12])=[O:10])(=[O:27])=[O:26])=[O:23])[CH3:20]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 5743389Methyl 2-aminobenzeneacetateHCID 12225100Ethyl (chlorosulfonyl)acetate

생성물 1

HCID 54096246HCID 54096246, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

To a solution of 82.7 g of methyl 2-aminophenylacetate (see Example l) in 1.2 l of toluene is added 42 ml of pyridine and the mixture is stirred at room temperature. To this mixture is added a solution of 93.2 g of ethoxycarbonylmethylsulfonyl chloride in 150 ml of toluene in a dropwise manner over a period of 30 minutes, maintaining the temperature of the reaction below 10° by means of an ice-water bath. After stirring at 0° for an additional 1 hour, the mixture is poured into 50 ml of ice-water, the organic layer is separated and washed with 150 ml of cold dilute hydrochloric acid followed by 150 ml of brine. The toluene extract is dried over anhydrous magnesium sulfate, filtered and the solvent evaporated under reduced pressure to yield methyl 2-(ethoxycarbonylmethylsulfonylamino)-phenylacetate as an oil which is used in the next step without further purification.

후처리

  1. temperaturemaintaining
  2. customthe temperature of the reaction below 10° by means of an ice-water bath
  3. stirringAfter stirring at 0° for an additional 1 hour
  4. customthe organic layer is separated
  5. washwashed with 150 ml of cold dilute hydrochloric acid
  6. extractionThe toluene extract
  7. dry with materialis dried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customthe solvent evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-d177707b35bd4ebe80a669a2384f7bbd
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04803197

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