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

HRID 2072422ノート

反応式

HRID 2072422 の反応式
[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

参加物

5

反応物 3

HCID 8471TriethylamineHCID 25072AminomatacilHCID 31297Methanesulfonyl chloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-24181135411a42c3a879bb8b177c34a6
出典データセット
uspto-grants-1977_09
特許番号
US04051254

反応ノート

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