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Hydrochloric Acid → HCID 22901902、化合物

HRID 1735989
ノート
印刷プレビュー

反応式

HRID 1735989 の反応式
C(OC([O:6][CH:7]1[C:12]2[CH:13]=[C:14]([S:16]([NH:19][C:20]([CH3:23])([CH3:22])[CH3:21])(=[O:18])=[O:17])[S:15][C:11]=2[S:10](=[O:25])(=[O:24])[N:9](C(OCC)C)[CH2:8]1)C)C.Cl>C1COCC1>[OH:6][CH:7]1[C:12]2[CH:13]=[C:14]([S:16]([NH:19][C:20]([CH3:21])([CH3:22])[CH3:23])(=[O:17])=[O:18])[S:15][C:11]=2[S:10](=[O:25])(=[O:24])[NH:9][CH2:8]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 19434048HCID 19434048、化合物

生成物 1

HCID 22901902HCID 22901902、化合物収率 75%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of the product from Step E (158 g, 0.325 mol), THF (700 mL) and 2N HCl (180 mL) were stirred at room temperature for 20 hr. After evaporating the THF, the aqueous mixture was cooled to 0° C. and sodium bicarbonate (50 g) was carefully added followed by water (400 mL) and ethyl acetate (500 mL). The two layers were separated and the aqueous layer was extracted with ethyl acetate (250 mL). The combined organic extracts were washed with brine, dried (MgSO4) and evaporated to give a foam which was triturated with methylene chloride (200 mL) to give a solid (81.7 g, 75%): mp 144°-147° C. Recrystallization of this solid from methylene chloride gave an off-white solid: mp 163°-165° C.

後処理

  1. customAfter evaporating the THF
  2. temperaturethe aqueous mixture was cooled to 0° C.
  3. additionsodium bicarbonate (50 g) was carefully added
  4. customThe two layers were separated
  5. extractionthe aqueous layer was extracted with ethyl acetate (250 mL)
  6. washThe combined organic extracts were washed with brine
  7. dry with materialdried (MgSO4)
  8. customevaporated
  9. customto give a foam which
  10. customwas triturated with methylene chloride (200 mL)

出典と根拠

ORDレコード
ord-f13e86aa1547499ea35d5ee6ccdd715c
出典データセット
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05538966

反応ノート

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