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

HRID 965554ノート

反応式

HRID 965554 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1d01a29dc1a84842b0924fbcd9f7b5ec
出典データセット
uspto-grants-1998_06
特許番号
US05773612

反応ノート

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