Hydrochloric Acid → HCID 178484861、化合物

HRID 630376ノート

反応式

HRID 630376 の反応式
[OH:1][C:2]([C:26]1[S:27][CH:28]=[CH:29][CH:30]=1)([C:21]1[S:22][CH:23]=[CH:24][CH:25]=1)[C:3]([O:5][C@H:6]1[CH2:11][CH2:10][C@H:9]([N:12](C(OC(C)(C)C)=O)[CH3:13])[CH2:8][CH2:7]1)=[O:4].Cl>O1CCOCC1>[OH:1][C:2]([C:21]1[S:22][CH:23]=[CH:24][CH:25]=1)([C:26]1[S:27][CH:28]=[CH:29][CH:30]=1)[C:3]([O:5][C@H:6]1[CH2:7][CH2:8][C@H:9]([NH:12][CH3:13])[CH2:10][CH2:11]1)=[O:4]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 178486063HCID 178486063、化合物2 回

生成物 1

HCID 178484861HCID 178484861、化合物収率 78%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of trans-4-[(tert-butoxycarbonyl)(methyl)amino]cyclohexyl hydroxy(di-2-thienyl)acetate (intermediate 4; 8.1 g, 0.01 mol) in dioxane (13.5 mL) was added hydrogen chloride 4M in dioxane (27 mL). The mixture was stirred at room temperature for 24 hours. The precipitate obtained was filtrated and washed with ether. The crude was dissolved in water and potassium carbonate was added until pH=8-9. The product was extracted with ethyl acetate and the organic layer was washed with brine, dried and evaporated to dryness giving the title compound as a white solid (78%).

後処理

  1. customThe precipitate obtained
  2. filtrationwas filtrated
  3. washwashed with ether
  4. dissolutionThe crude was dissolved in water
  5. additionpotassium carbonate was added until pH=8-9
  6. extractionThe product was extracted with ethyl acetate
  7. washthe organic layer was washed with brine
  8. customdried
  9. customevaporated to dryness

出典と根拠

ORDレコード
ord-2d8c6416cbac4bb49c7ede0042cd467f
出典データセット
uspto-grants-2016_04
特許番号
US09315463B2

反応ノート

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