Hydrochloric Acid → HCID 58447828、化合物

HRID 592253ノート

反応式

HRID 592253 の反応式
[S:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:12]=[CH:11][C:10]([CH:13](C(OCC)=O)[C:14]([O:16]CC)=[O:15])=[CH:9][CH:8]=2)[CH2:3][CH2:2]1.[OH-].[Na+].Cl.C([O-])([O-])=O.[Na+].[Na+]>O1CCOCC1.O>[S:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:12]=[CH:11][C:10]([CH2:13][C:14]([OH:16])=[O:15])=[CH:9][CH:8]=2)[CH2:3][CH2:2]1

参加物

7

反応条件

温度
88 °C

実験手順

2-(6-Thiomorpholinopyridin-3-yl)malonate 219-3 (564 mg, 1.67 mmol) was stirred with NaOH (334 mg, 8.35 mmol) in dioxane (5 ml) and water (5 ml) for 4 hours. HCl solution was added to adjust the pH around 1 and the reaction mixture heated at 88° C. for 1 hour. Then Na2CO3 was used to adjust the pH to around 4 before the solvents were evaporated. The residue was extracted with ethyl acetate and the organic extraction dried over Na2SO4 and concentrated by rotary evaporation. Purification with reverse phase HPLC afforded 2-(6-thiomorpholinopyridin-3-yl)acetic acid 219-4.

後処理

  1. customwere evaporated
  2. extractionThe residue was extracted with ethyl acetate
  3. extractionthe organic extraction
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated by rotary evaporation
  6. customPurification with reverse phase HPLC

出典と根拠

ORDレコード
ord-92d65d24ed634bf588eba7e094974b5c
出典データセット
uspto-grants-2016_01
特許番号
US09238646B2

反応ノート

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