Hydrochloric Acid → phenyl N-(2-biphenylylsulfonyl)carbamate

HRID 745857

反応式

HRID 745857 の反応式
[H-].[Na+].[C:3]1([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[S:15]([NH2:18])(=[O:17])=[O:16])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:19](=O)([O:27]C1C=CC=CC=1)[O:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.Cl>CN(C)C=O>[C:9]1([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[S:15]([NH:18][C:19](=[O:27])[O:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)(=[O:16])=[O:17]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7597Diphenyl carbonateHCID 24758Sodium hydrideHCID 123715202-Phenylbenzene-1-sulfonamide

生成物 1

HCID 13590973phenyl N-(2-biphenylylsulfonyl)carbamate収率 99.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

Sodium hydride (2.6 g) was added to dry dimethylformamide (200 ml), and at less than 10° C., a solution of 2-phenylbenzenesulfonamide (23.3 g) in dimethylformamide (50 ml) was added. The mixture was then stirred at room temperature for 1 hour, and diphenyl carbonate (21.4 g) was added at room temperature. The mixture was further stirred at room temperature for 1 hour. Then, after the whole mixture was added to ice water, the mixture was acidified with hydrochloric acid and extracted with ethyl acetate. The organic layer was dehydrated, and ethyl acetate was distilled off under reduced pressure to give phenyl N-(2-biphenylylsulfonyl)carbamate (35 g) as a solidified desired compound represented by the following formula. mp. 114°-117° C. ##STR11##

後処理

  1. stirringThe mixture was further stirred at room temperature for 1 hour
  2. extractionextracted with ethyl acetate
  3. distillationethyl acetate was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-b451aa9c8b1c4b67abab6a6e4f66cdaa
出典データセット
uspto-grants-1986_07
特許番号
US04600792

関連ノート

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