Hydroxyamine hydrochloride → HCID 25009625, 화합물

HRID 14992노트

반응식

HRID 14992 반응식
[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

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 24864113HCID 24864113, 화합물

생성물 1

HCID 25009625HCID 25009625, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1cb44697a2c046d5a471bac03c1dbbb1
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732440B2

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