Hydrochloric Acid → HCID 67259494, 화합물

HRID 1476663노트

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HRID 1476663 반응식
[CH2:1]([O:3][C:4]1[C:13]([O:14][CH3:15])=[CH:12][C:11]2[C:10]([C:16]3[CH:25]=[CH:24][C:19]([C:20]([O:22]C)=[O:21])=[CH:18][CH:17]=3)=[N:9][C@@H:8]3[CH2:26][CH2:27][S:28](=[O:31])(=[O:30])[CH2:29][C@@H:7]3[C:6]=2[CH:5]=1)[CH3:2].[OH-].[Na+].Cl>O1CCOCC1>[CH2:1]([O:3][C:4]1[C:13]([O:14][CH3:15])=[CH:12][C:11]2[C:10]([C:16]3[CH:25]=[CH:24][C:19]([C:20]([OH:22])=[O:21])=[CH:18][CH:17]=3)=[N:9][C@@H:8]3[CH2:26][CH2:27][S:28](=[O:30])(=[O:31])[CH2:29][C@@H:7]3[C:6]=2[CH:5]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67257612HCID 67257612, 화합물2회

생성물 1

HCID 67259494HCID 67259494, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of methyl 4-[(4aR,10bR)-9-ethoxy-8-methoxy-2,2-dioxido-3,4,4a,10b-tetrahydro-1H-thiopyrano[4,3-c]isoquinolin-6-yl]benzoate (380 mg; compound C5) in 1,4-dioxane (10 ml) is treated with an 2 M aqueous solution of sodium hydroxide (1 ml) and the reaction solution is stirred for about 20 h at 45° C. to 50° C. The solution is allowed to come to RT and afterwards a 2 M aqueous solution of hydrogen chloride (1 ml) is added. The mixture is stirred for 20 min at RT, filtered and the filtrate is evaporated to dryness in vacuo. Subsequently, the residue is treated with DCM (30 ml) and the resulting suspension is filtered. The solvent is removed in vacuo to yield the title compound as a solid.

후처리

  1. customto come to RT
  2. stirringThe mixture is stirred for 20 min at RT
  3. filtrationfiltered
  4. customthe filtrate is evaporated to dryness in vacuo
  5. additionSubsequently, the residue is treated with DCM (30 ml)
  6. filtrationthe resulting suspension is filtered
  7. customThe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-eca98a8b7fda4baab1d2110544905150
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09018175B2

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