Hydrochloric Acid → HCID 71079543, 화합물

HRID 337213노트

반응식

HRID 337213 반응식
C(OC(=O)[NH:7][CH:8]1[CH2:13][CH2:12][N:11]([S:14]([C:17]2[CH:22]=[CH:21][C:20]([N:23]([CH3:32])[C:24]([CH:26]3[CH2:31][CH2:30][O:29][CH2:28][CH2:27]3)=[O:25])=[CH:19][CH:18]=2)(=[O:16])=[O:15])[CH2:10][CH2:9]1)(C)(C)C.Cl>O1CCOCC1>[NH2:7][CH:8]1[CH2:9][CH2:10][N:11]([S:14]([C:17]2[CH:18]=[CH:19][C:20]([N:23]([CH3:32])[C:24]([CH:26]3[CH2:31][CH2:30][O:29][CH2:28][CH2:27]3)=[O:25])=[CH:21][CH:22]=2)(=[O:15])=[O:16])[CH2:12][CH2:13]1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 71060228(1-{4-[Methyl-(tetrahydro-pyran-4-carbonyl)-amino]-benzenesulfonyl}-piperidin-4-yl)-carbamic acid tert-butyl ester

생성물 1

HCID 71079543HCID 71079543, 화합물수율 111.4%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

[(1-{4-[Methyl-(tetrahydro-pyran-4-carbonyl)-amino]-benzenesulfonyl}-piperidin-4-yl)-carbamic acid tert-butyl ester (0.17 g, 0.4 mmol) was suspended in a 4M solution of HCl in Dioxane (5 ml). The resulting suspension was stirred at room temperature for 3 hours. After this time the solution was concentrated under vacuum, then azeotroped with methanol and suspended in diethyl ether. The resulting solid precipitate was then collected by filtration, washed with diethyl ether and dried under vacuum to afford the title compound (0.17 g, Quantitative yield) as a white solid. Tr=1.20 min, m/z (ES+) (M+H)+ 382.

후처리

  1. concentrationAfter this time the solution was concentrated under vacuum
  2. customazeotroped with methanol
  3. filtrationThe resulting solid precipitate was then collected by filtration
  4. washwashed with diethyl ether
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-a26f90ed91a547dd8607b918e78f18dc
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889716B2

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