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

HRID 899148노트

반응식

HRID 899148 반응식
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]

참가 물질

4

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-08cfc95d1dc8430f8693423a8bc4e9b0
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07354917B2

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