N-Butyl-N-(2-(2-(5-hydroxy-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazin-8-yl)ethylamino)ethyl)-3-(3-(2-(4-(2-isopropylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)ethyl)phenethoxy)propanamide monosulphate salt → N-Butyl-N-(2-(2-(5-hydroxy-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazin-8-yl)ethylamino)ethyl)-3-(3-(2-(4-(2-isopropylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)ethyl)phenethoxy)propanamide

HRID 1255336노트

반응식

HRID 1255336 반응식
S(O)(O)(=O)=O.[CH2:6]([N:10]([CH2:47][CH2:48][NH:49][CH2:50][CH2:51][C:52]1[C:57]2[O:58][CH2:59][C:60](=[O:62])[NH:61][C:56]=2[C:55]([OH:63])=[CH:54][CH:53]=1)[C:11](=[O:46])[CH2:12][CH2:13][O:14][CH2:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([CH2:23][CH2:24][N:25]2[CH2:45][CH2:44][C:28]3([O:33][CH2:32][CH2:31][N:30]([C:34]([C:36]4[N:37]=[C:38]([CH:41]([CH3:43])[CH3:42])[S:39][CH:40]=4)=[O:35])[CH2:29]3)[CH2:27][CH2:26]2)[CH:18]=1)[CH2:7][CH2:8][CH3:9]>C(Cl)Cl.CO>[CH2:6]([N:10]([CH2:47][CH2:48][NH:49][CH2:50][CH2:51][C:52]1[C:57]2[O:58][CH2:59][C:60](=[O:62])[NH:61][C:56]=2[C:55]([OH:63])=[CH:54][CH:53]=1)[C:11](=[O:46])[CH2:12][CH2:13][O:14][CH2:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([CH2:23][CH2:24][N:25]2[CH2:45][CH2:44][C:28]3([O:33][CH2:32][CH2:31][N:30]([C:34]([C:36]4[N:37]=[C:38]([CH:41]([CH3:42])[CH3:43])[S:39][CH:40]=4)=[O:35])[CH2:29]3)[CH2:27][CH2:26]2)[CH:18]=1)[CH2:7][CH2:8][CH3:9]

참가 물질

3

반응물 1

HCID 86651693N-Butyl-N-(2-(2-(5-hydroxy-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazin-8-yl)ethylamino)ethyl)-3-(3-(2-(4-(2-isopropylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)ethyl)phenethoxy)propanamide monosulphate salt

생성물 1

HCID 51036603N-Butyl-N-(2-(2-(5-hydroxy-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazin-8-yl)ethylamino)ethyl)-3-(3-(2-(4-(2-isopropylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)ethyl)phenethoxy)propanamide

시약·촉매·용매 1

HCID 21226129Dichloromethane methanol용매

실험 절차

N-Butyl-N-(2-(2-(5-hydroxy-3-oxo-3,4-dihydro-2H-benzo[b][1,4]oxazin-8-yl)ethylamino)ethyl)-3-(3-(2-(4-(2-isopropylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)ethyl)phenethoxy)propanamide Sulphate salt Modification A (Example 34a) (1.73 g) was dissolved in DCM/methanol, filtered and evaporated to dryness. The resultant gum was partitioned between sat aq bicarb (100 mL) and freshly distilled MeTHF (150 mL) and the mixture stirred vigorously for 10 mins. The organic layer was separated, washed with fresh sodium bicarbonate (×2), dried over sodium sulphate, filtered and evaporated under reduced pressure to give the title compound as a foam. Yield 1.2 g.

후처리

  1. filtrationfiltered
  2. customevaporated to dryness
  3. customThe resultant gum was partitioned
  4. customThe organic layer was separated
  5. washwashed with fresh sodium bicarbonate (×2)
  6. dry with materialdried over sodium sulphate
  7. filtrationfiltered
  8. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-9ed9b2720d69428785a33edb6e6f90a0
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455483B2

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