Sodium Hydroxide → 1-(Morpholin-4-ylsulfonyl)piperidine-4-carboxylic acid

HRID 2381180ノート

反応式

HRID 2381180 の反応式
C([O:3][C:4]([CH:6]1[CH2:11][CH2:10][N:9]([S:12]([N:15]2[CH2:20][CH2:19][O:18][CH2:17][CH2:16]2)(=[O:14])=[O:13])[CH2:8][CH2:7]1)=[O:5])C.[OH-].[Na+]>CO>[N:15]1([S:12]([N:9]2[CH2:10][CH2:11][CH:6]([C:4]([OH:5])=[O:3])[CH2:7][CH2:8]2)(=[O:14])=[O:13])[CH2:16][CH2:17][O:18][CH2:19][CH2:20]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 3422241HCID 3422241、化合物

生成物 1

HCID 32397731-(Morpholin-4-ylsulfonyl)piperidine-4-carboxylic acid収率 79.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
85 °C

実験手順

1-(Morpholine-4-sulfonyl)-piperidine-4-carboxylic acid ethyl ester (1.9 g) dissolved in methanol (80 ml) was treated at RT with 2M NaOH (15.5 ml) and the mixture was then heated at 85° C. for 12 h. The solvent was then evaporated off, the residue partitioned between methylene chloride and 1N HCL, the layers were separated and the organic layer washed with 2M aqueous KHCO3, dried over Na2SO4 and concentrated in vacuo to give 1-(morpholine-4-sulfonyl)-piperidine-4-carboxylic acid (1.37 g) as a white solid. MS (ESI): 277.08 ([M-H]−).

後処理

  1. customThe solvent was then evaporated off
  2. customthe residue partitioned between methylene chloride and 1N HCL
  3. customthe layers were separated
  4. washthe organic layer washed with 2M aqueous KHCO3
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3ec7bd2d5457490db0cd26bd40e48906
出典データセット
uspto-grants-2012_09
特許番号
US08258158B2

反応ノート

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