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Lithium Hydroxide → 3-[[[3-(4-Acetyl-3-hydroxy-2-propylphenoxy)-2-hydroxypropyl]thio]methyl]-1-oxa-4-thiaspiro[4.4]nonane-7-acetic acid

HRID 1608281
ノート
印刷プレビュー

反応式

HRID 1608281 の反応式
[C:1]([C:4]1[CH:31]=[CH:30][C:7]([O:8][CH2:9][CH:10]([OH:29])[CH2:11][S:12][CH2:13][CH:14]2[S:18][C:17]3([CH2:22][CH2:21][CH:20]([CH2:23][C:24]([O:26]CC)=[O:25])[CH2:19]3)[O:16][CH2:15]2)=[C:6]([CH2:32][CH2:33][CH3:34])[C:5]=1[OH:35])(=[O:3])[CH3:2].[Li+].[OH-]>C(O)C>[C:1]([C:4]1[CH:31]=[CH:30][C:7]([O:8][CH2:9][CH:10]([OH:29])[CH2:11][S:12][CH2:13][CH:14]2[S:18][C:17]3([CH2:22][CH2:21][CH:20]([CH2:23][C:24]([OH:26])=[O:25])[CH2:19]3)[O:16][CH2:15]2)=[C:6]([CH2:32][CH2:33][CH3:34])[C:5]=1[OH:35])(=[O:3])[CH3:2]
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 3939Lithium HydroxideHCID 19849026Ethyl 3-[[[3-(4-acetyl-3-hydroxy-2-propylphenoxy)-2-hydroxypropyl]thio]methyl]-1-oxa-4-thiaspiro[4.4]nonane-7-acetate

生成物 1

HCID 198490283-[[[3-(4-Acetyl-3-hydroxy-2-propylphenoxy)-2-hydroxypropyl]thio]methyl]-1-oxa-4-thiaspiro[4.4]nonane-7-acetic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The product of Example 10 is saponified according to the procedure of Example 2 using 5.3 g (10 mmol) of the above ester and 2M LiOH solution (12.5 ml, 2.5 eq.) in ethanol (50 ml). After stirring overnight at room temperature, the solvent is removed in vacuo and the residue diluted with water. After acidification to pH 2.5 with 0.5N KHSO4, the mixture is extracted with ethyl acetate and dried over magnesium sulfate. The drying agent is filtered and the filtrate is concentrated in vacuo. Further drying of the resultant residue at 60° (0.5 torr) gives the titled compound.

後処理

  1. customthe solvent is removed in vacuo
  2. additionthe residue diluted with water
  3. extractionAfter acidification to pH 2.5 with 0.5N KHSO4, the mixture is extracted with ethyl acetate
  4. dry with materialdried over magnesium sulfate
  5. filtrationThe drying agent is filtered
  6. concentrationthe filtrate is concentrated in vacuo
  7. dry with materialFurther drying of the resultant residue at 60° (0.5 torr)

出典と根拠

ORDレコード
ord-8fe711a2d08f4f1e8d7a7f70aafeceb0
出典データセット
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04870098

反応ノート

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