Hydrochloric Acid → HCID 58447828, 화합물

HRID 592253노트

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HRID 592253 반응식
[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

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 58447952HCID 58447952, 화합물

생성물 1

HCID 58447828HCID 58447828, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

반응 조건

온도
88 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-92d65d24ed634bf588eba7e094974b5c
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238646B2

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