Water → 3-Acetamido-5-chloro-3-(2-chlorophenyl)-1,3-dihydro-1-(2-methoxy-4-nitrobenzenesulfonyl)indol-2-one

HRID 234506노트

반응식

HRID 234506 반응식
[NH2:1][C:2]1([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[Cl:33])[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([Cl:11])[CH:9]=2)[N:4]([S:12]([C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][C:16]=2[O:24][CH3:25])(=[O:14])=[O:13])[C:3]1=[O:26].[C:34](Cl)(=[O:36])[CH3:35].O>N1C=CC=CC=1>[C:34]([NH:1][C:2]1([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[Cl:33])[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([Cl:11])[CH:9]=2)[N:4]([S:12]([C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][C:16]=2[O:24][CH3:25])(=[O:13])=[O:14])[C:3]1=[O:26])(=[O:36])[CH3:35]

참가 물질

5

반응물 3

HCID 962WaterHCID 6367Acetyl chlorideHCID 190765153-Amino-5-chloro-3-(2-chlorophenyl)-1,3-dihydro-1-(2-methoxy-4-nitrobenzenesulfonyl)indol-2-one

생성물 1

HCID 190764193-Acetamido-5-chloro-3-(2-chlorophenyl)-1,3-dihydro-1-(2-methoxy-4-nitrobenzenesulfonyl)indol-2-one

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of 2.8 g of the compound obtained in EXAMPLE 16 in 10 ml of pyridine is cooled in an ice bath and 0.51 ml of acetyl chloride is added. The reaction medium is stirred for 3 hours at RT and poured into water. It is extracted with AcOEt, washed with water and with a 5% solution of potassium hydrogensulfate, dried over sodium sulfate and evaporated under vacuum. The residue is taken up with DCM and the precipitate formed is filtered off to give 2.8 g of the expected product, a sample of which is crystallized from an MeOH/iso ether mixture. M.p.=205°-210° C.

후처리

  1. extractionIt is extracted with AcOEt
  2. washwashed with water and with a 5% solution of potassium hydrogensulfate
  3. dry with materialdried over sodium sulfate
  4. customevaporated under vacuum
  5. customthe precipitate formed
  6. filtrationis filtered off

출처 및 근거

ORD 기록
ord-c19adfc1efb543df87616ef1142563ef
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05594023

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