Sodium Hydroxide → 6-(N-Boc-N-2-picolylaminomethyl)nicotinic Acid

HRID 11846

반응식

HRID 11846 반응식
[C:1]([N:8]([CH2:16][C:17]1[CH:26]=[CH:25][C:20]([C:21]([O:23]C)=[O:22])=[CH:19][N:18]=1)[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[OH-].[Na+]>CO.C1COCC1>[C:1]([N:8]([CH2:16][C:17]1[CH:26]=[CH:25][C:20]([C:21]([OH:23])=[O:22])=[CH:19][N:18]=1)[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2]

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 21973709Methyl 6-(N-Boc-N-2-picolylaminomethyl)nicotinate

생성물 1

HCID 219736636-(N-Boc-N-2-picolylaminomethyl)nicotinic Acid수율 82.3%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

The compound obtained in Example 12-2 (351.3 mg) was dissolved in methanol (3.5 ml) and THF (3.5 ml). After the addition of 1 mol/l aqueous solution of sodium hydroxide (3.5 ml), the mixture was stirred for 2 hours at room temperature. After the reaction, the solvent was removed by distillation. The residue was dissolved in distilled water (1.2 ml) and aqueous solution of hydrochloric acid (1 mol/l) was added to adjust the pH to 4. The mixture was extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate. The solvent was removed by distillation to obtain the target compound (277.9 mg) as a white solid.

후처리

  1. customAfter the reaction
  2. customthe solvent was removed by distillation
  3. dissolutionThe residue was dissolved in distilled water (1.2 ml)
  4. additionaqueous solution of hydrochloric acid (1 mol/l) was added
  5. extractionThe mixture was extracted with chloroform
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. customThe solvent was removed by distillation

출처 및 근거

ORD 기록
ord-a78d72c6fe744272bcfd3a458c7ab371
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098215B2

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