Sodium Acetate → 6-(5-Aminoisoxazol-3-yl)-3-(2,4-dichlorophenyl)-1,9-dimethyl-1,9-dihydropyrido[2,3-b]indol-2-one

HRID 559152ノート

反応式

HRID 559152 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[C:27](=[O:28])[N:26]([CH3:29])[C:12]2[N:13]([CH3:25])[C:14]3[C:19]([C:11]=2[CH:10]=1)=[CH:18][C:17]([C:20](=O)[CH2:21][C:22]#[N:23])=[CH:16][CH:15]=3.C([O-])(=O)C.[Na+].Cl.[OH:36][NH-:37]>C(Cl)Cl.CO>[NH2:23][C:22]1[O:36][N:37]=[C:20]([C:17]2[CH:18]=[C:19]3[C:14](=[CH:15][CH:16]=2)[N:13]([CH3:25])[C:12]2[N:26]([CH3:29])[C:27](=[O:28])[C:9]([C:3]4[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=4[Cl:1])=[CH:10][C:11]3=2)[CH:21]=1

参加物

6

反応物 3

HCID 517045Sodium AcetateHCID 669980453-[3-(2,4-dichlorophenyl)-1,9-dimethyl-2-oxo-2,9-dihydro-1H-pyrido[2,3-b]indol-6-yl]-3-oxopropionitrileHCID 178479582HCID 178479582、化合物

生成物 1

HCID 669984026-(5-Aminoisoxazol-3-yl)-3-(2,4-dichlorophenyl)-1,9-dimethyl-1,9-dihydropyrido[2,3-b]indol-2-one

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
50 °C

実験手順

A solution containing 300 mg (0.707 mmol) of compound 3-[3-(2,4-dichlorophenyl)-1,9-dimethyl-2-oxo-2,9-dihydro-1H-pyrido[2,3-b]indol-6-yl]-3-oxopropionitrile from Example 20A, 238 mg (2.9 mmol) of sodium acetate and 152 mg (2.2 mmol) of hydroxylamide hydrochloride in 4 ml of CH2Cl2 and 4 ml of MeOH is stirred at 50° C. for 24 h and then at ambient temperature for 18 h. The reaction medium is concentrated by adsorbing it onto silica, and purification is carried out on a silica column, elution being carried out with EtOAc/20% cyclohexane and then 100% EtOAc.

後処理

  1. waitat ambient temperature for 18 h
  2. concentrationThe reaction medium is concentrated
  3. customonto silica, and purification
  4. washis carried out on a silica column, elution

出典と根拠

ORDレコード
ord-573976d6f988410b93dfa9f441af50f7
出典データセット
uspto-grants-2011_11
特許番号
US08063061B2

反応ノート

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