Hydrochloric Acid → HCID 67259494、化合物

HRID 1476663ノート

反応式

HRID 1476663 の反応式
[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]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 67257612HCID 67257612、化合物2 回

生成物 1

HCID 67259494HCID 67259494、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-eca98a8b7fda4baab1d2110544905150
出典データセット
uspto-grants-2015_04
特許番号
US09018175B2

反応ノート

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