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Hydrochloric Acid → HCID 10019238、化合物

HRID 1494121
ノート
印刷プレビュー

反応式

HRID 1494121 の反応式
O1CCCCC1[O:7][CH2:8][CH2:9][CH2:10][CH2:11][CH:12]([CH2:20][CH2:21][CH2:22][C:23]1[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=1)[S:13][CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16].Cl>O1CCCC1>[OH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH:12]([CH2:20][CH2:21][CH2:22][C:23]1[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=1)[S:13][CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16]
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 Acid2 回HCID 10001566HCID 10001566、化合物

生成物 1

HCID 10019238HCID 10019238、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 0.241 g (0.59 mmol) ethyl 8-(2-tetrahydropyranyloxy)-4-[3-(3-pyridyl)propyl]-3thia-octanoate in 1 ml tetrahydrofuran is added 1 mL of 1N hydrochloric acid. After stirring for 1 hour at room temperature, thin layer chromatography indicates incomplete conversion. Another 0.35 mL of 6N hydrochloric acid is added and the mixture is stirred for 1 hour. The pH of the reaction mixture is then adjusted to 8.0 and the resulting solution is extracted with methylene chloride. The organic layer is washed with brine, dried, filtered and evaporated to give yellow oil which is purified by preparative thin layer chromatography over silica gel using ether/ethyl acetate (4:1) as eluent to give ethyl 8-hydroxy-4-[3-(3-pyridyl)propyl]-3-thia-octanoate; IR (CH2Cl2) 3679, 1730 cm-1.

後処理

  1. stirringthe mixture is stirred for 1 hour
  2. extractionthe resulting solution is extracted with methylene chloride
  3. washThe organic layer is washed with brine
  4. customdried
  5. filtrationfiltered
  6. customevaporated
  7. customto give yellow oil which
  8. customis purified by preparative thin layer chromatography over silica gel

出典と根拠

ORDレコード
ord-ca52e10055c546ada0da9919ea286f40
出典データセット
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05025025

反応ノート

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