Triethylamine → 3-methyl-4-(methanesulfonamido)phenyl N-methylcarbamate

HRID 2072422노트

반응식

HRID 2072422 반응식
[CH3:1][NH:2][C:3](=[O:13])[O:4][C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[C:7]([CH3:12])[CH:6]=1.C(N(CC)CC)C.[CH3:21][S:22](Cl)(=[O:24])=[O:23]>C1C=CC=CC=1>[CH3:1][NH:2][C:3](=[O:13])[O:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][S:22]([CH3:21])(=[O:24])=[O:23])=[C:7]([CH3:12])[CH:6]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 25072AminomatacilHCID 31297Methanesulfonyl chloride

생성물 1

HCID 214093123-methyl-4-(methanesulfonamido)phenyl N-methylcarbamate

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A flask was charged with 3-methyl-4-aminophenyl N-methylcarbamate (3.0g., 0.0166 mole), triethylamine (1.83g., 0.018 mole, 2.53 ml.) and about 100 ml. of benzene. To this slurry was added methanesulfonyl chloride and after one hour at reflux the mixture was cooled and filtered. The solids were stirred vigorously with water to dissolve any residual by-product triethylamine hydrochloride. Refiltration and drying gave 2.3g. of the desired product (m.p. 167°-69° C.).

후처리

  1. temperatureafter one hour at reflux the mixture
  2. temperaturewas cooled
  3. filtrationfiltered
  4. dissolutionto dissolve any residual by-product triethylamine hydrochloride
  5. customRefiltration and drying
  6. customgave 2.3g

출처 및 근거

ORD 기록
ord-24181135411a42c3a879bb8b177c34a6
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04051254

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