Hydroxyamine hydrochloride → HCID 25009625、化合物

HRID 14992ノート

反応式

HRID 14992 の反応式
[CH3:1][N:2]1[C:15]2[CH:14]=[C:13]([CH:16]([CH2:26][CH:27]3[CH2:32][CH2:31][C:30](=O)[CH2:29][CH2:28]3)[C:17]([NH:19][C:20]3[CH:24]=[CH:23][N:22]([CH3:25])[N:21]=3)=[O:18])[CH:12]=[CH:11][C:10]=2[S:9](=[O:35])(=[O:34])[C:8]2[C:3]1=[CH:4][CH:5]=[CH:6][CH:7]=2.Cl.[NH2:37][OH:38]>CO>[OH:38][N:37]=[C:30]1[CH2:31][CH2:32][CH:27]([CH2:26][CH:16]([C:13]2[CH:12]=[CH:11][C:10]3[S:9](=[O:34])(=[O:35])[C:8]4[C:3](=[CH:4][CH:5]=[CH:6][CH:7]=4)[N:2]([CH3:1])[C:15]=3[CH:14]=2)[C:17]([NH:19][C:20]2[CH:24]=[CH:23][N:22]([CH3:25])[N:21]=2)=[O:18])[CH2:28][CH2:29]1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 24864113HCID 24864113、化合物

生成物 1

HCID 25009625HCID 25009625、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

67 mg of 2-(10-methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-N-(1-methyl-1H-pyrazol-3-yl)-3-(4-oxocyclohexyl)propionamide and 14 mg of hydroxylamine hydrochloride are dissolved in 13 ml of methanol and heated at the boil under reflux for three hours. The methanol is then removed under reduced pressure, and the resulting residue is taken up in a mixture of 20 ml of ethyl acetate and 10 ml of water. The organic phase is washed twice with in each case 10 ml of water, dried over MgSO4, concentrated under reduced pressure and then lyophilized. This gives 49 mg of 3-(4-hydroxyiminocyclohexyl)-2-(10-methyl-5,5-dioxo-5,10-dihydrophenothiazin-2-yl)-N-(1-methyl-1H-pyrazol-3-yl)propionamide.

後処理

  1. temperatureheated at the boil
  2. temperatureunder reflux for three hours
  3. customThe methanol is then removed under reduced pressure
  4. additionthe resulting residue is taken up in a mixture of 20 ml of ethyl acetate and 10 ml of water
  5. washThe organic phase is washed twice with in each case 10 ml of water
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1cb44697a2c046d5a471bac03c1dbbb1
出典データセット
uspto-grants-2010_06
特許番号
US07732440B2

反応ノート

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