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 1255336ノート

反応式

HRID 1255336 の反応式
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]

参加物

3

反応物 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

生成物 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

試薬・触媒・溶媒 1

HCID 21226129Dichloromethane methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9ed9b2720d69428785a33edb6e6f90a0
出典データセット
uspto-grants-2013_06
特許番号
US08455483B2

反応ノート

読み込み中…