Water → HCID 71238166、化合物

HRID 1846659ノート

反応式

HRID 1846659 の反応式
C([O:3][C:4](=[O:30])[CH2:5][CH:6]1[CH2:11][CH2:10][N:9]([C:12]2[C:17]([NH:18][C:19](=[O:27])[C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[CH:21]=3)=[CH:16][C:15]([C:28]#[N:29])=[CH:14][N:13]=2)[CH2:8][CH2:7]1)C.O.[OH-].[Li+]>C1COCC1.CO>[Cl:26][C:22]1[CH:21]=[C:20]([CH:25]=[CH:24][CH:23]=1)[C:19]([NH:18][C:17]1[C:12]([N:9]2[CH2:8][CH2:7][CH:6]([CH2:5][C:4]([OH:30])=[O:3])[CH2:11][CH2:10]2)=[N:13][CH:14]=[C:15]([C:28]#[N:29])[CH:16]=1)=[O:27]

参加物

6

反応物 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 71238641HCID 71238641、化合物

生成物 1

HCID 71238166HCID 71238166、化合物収率 80%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 0.047 g (0.11 mmol) of [3′-(3-chloro-benzoylamino)-5′-cyano-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-4-yl]-acetic acid ethyl ester in a mixture of THF (5 mL) and MeOH (2 mL) is added water (1 mL) and 0.013 g (0.55 mmol) of lithium hydroxide. The reaction mixture is stirred at room temperature for three days. The solvent is removed under reduced pressure and the residue is taken back up into water. The pH of the resulting aqueous solution is adjusted to approximately pH2 by adding concentrated hydrochloric acid which results in a solid precipitating from solution. The formed precipitate is collected by filtration, washed with water, and dried under vacuum to give 0.035 g (80%) of [3′-(3-chloro-benzoylamino)-5′-cyano-3,4,5,6-tetrahydro-2H-[1,2′]bipyridinyl-4-yl]-acetic acid as yellow solid.

後処理

  1. customThe solvent is removed under reduced pressure
  2. additionby adding concentrated hydrochloric acid which
  3. customresults in a solid
  4. customprecipitating from solution
  5. filtrationThe formed precipitate is collected by filtration
  6. washwashed with water
  7. customdried under vacuum

出典と根拠

ORDレコード
ord-049a5036e8364081aeb2d67c41bbe84c
出典データセット
uspto-grants-2015_02
特許番号
US08952004B2

反応ノート

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