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

HRID 745857

반응식

HRID 745857 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 13590973phenyl N-(2-biphenylylsulfonyl)carbamate수율 99.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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##

후처리

  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

출처 및 근거

ORD 기록
ord-b451aa9c8b1c4b67abab6a6e4f66cdaa
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04600792

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