Hydrochloric Acid → N-[2-(4-Cyanophenoxy)ethyl]-N-[2-(9-oxa-3,7-diazabicyclo[3.3.1]non-3-yl)ethyl]methanesulfonamide

HRID 899148ノート

反応式

HRID 899148 の反応式
Cl.C(OC([N:9]1[CH2:16][CH:15]2[O:17][CH:11]([CH2:12][N:13]([CH2:18][CH2:19][N:20]([CH2:25][CH2:26][O:27][C:28]3[CH:33]=[CH:32][C:31]([C:34]#[N:35])=[CH:30][CH:29]=3)[S:21]([CH3:24])(=[O:23])=[O:22])[CH2:14]2)[CH2:10]1)=O)(C)(C)C>O1CCOCC1>[C:34]([C:31]1[CH:30]=[CH:29][C:28]([O:27][CH2:26][CH2:25][N:20]([CH2:19][CH2:18][N:13]2[CH2:14][CH:15]3[O:17][CH:11]([CH2:10][NH:9][CH2:16]3)[CH2:12]2)[S:21]([CH3:24])(=[O:23])=[O:22])=[CH:33][CH:32]=1)#[N:35]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 690747607-(2-{[2-(4-Cyanophenoxy)ethyl]methanesulfonylamino}ethyl)-9-oxa-3,7-diazabicyclo[3.3.1]nonane-3-carboxylic acid tert-butyl ester

生成物 1

HCID 69072689N-[2-(4-Cyanophenoxy)ethyl]-N-[2-(9-oxa-3,7-diazabicyclo[3.3.1]non-3-yl)ethyl]methanesulfonamide

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To a saturated solution of HCl(g) in dioxane (100 mL) was added 7-(2-{[2-(4-cyanophenoxy)ethyl]methanesulfonylamino}ethyl)-9-oxa-3,7-diaza-bicyclo[3.3.1]nonane-3-carboxylic acid tert-butyl ester (3.5 g, 0.0070 mol; see step (i) above), after which the reaction was stirred for 1 h. On completion of the reaction (as determined by TLC), dioxane was decanted and product (semi-solid) dissolved in methanol (25 mL). After concentrating the methanol, dry ether (50 mL) was added and the solvent was again concentrated. This was repeated twice and finally the product was dried under high vacuum. Yield: 3.0 g (99%).

後処理

  1. customwas decanted
  2. dissolutionproduct (semi-solid) dissolved in methanol (25 mL)
  3. concentrationAfter concentrating the methanol, dry ether (50 mL)
  4. additionwas added
  5. concentrationthe solvent was again concentrated
  6. customfinally the product was dried under high vacuum

出典と根拠

ORDレコード
ord-08cfc95d1dc8430f8693423a8bc4e9b0
出典データセット
uspto-grants-2008_04
特許番号
US07354917B2

反応ノート

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