Methanol → 4-[N-Boc-N-(pyridin-2-ylmethyl)aminomethyl]benzoic acid

HRID 11836노트

반응식

HRID 11836 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][CH: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].CO.[OH-].[Na+]>C1COCC1>[C:1]([N:8]([CH2:16][C:17]1[CH:18]=[CH:19][C:20]([C:21]([OH:23])=[O:22])=[CH:25][CH:26]=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 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 21973580methyl 4-[N-Boc-N-(pyridin-2-ylmethyl)aminomethyl]benzoate

생성물 1

HCID 219736504-[N-Boc-N-(pyridin-2-ylmethyl)aminomethyl]benzoic acid수율 63.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

The compound obtained in Example 1-1 (200.6 mg) was added with methanol (2 ml), THF (2 ml), and 1 mol/l aqueous solution of sodium hydroxide (2 ml), and the mixture was stirred for one day at room temperature. After the completion of the reaction, the solvent was removed by distillation and water (5 ml) was added. Aqueous solution of hydrochloric acid (1 mol/l) was added dropwise to the resulting solution to adjust the pH to 3. The deposited crystals were collected by filtration and dried to obtain the title compound (123.2 mg) as colorless crystals.

후처리

  1. customAfter the completion of the reaction
  2. customthe solvent was removed by distillation and water (5 ml)
  3. additionwas added
  4. additionAqueous solution of hydrochloric acid (1 mol/l) was added dropwise to the resulting solution
  5. filtrationThe deposited crystals were collected by filtration
  6. customdried

출처 및 근거

ORD 기록
ord-d2bf217eddca4257ae51da4d5cb2c928
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098215B2

반응 노트

불러오는 중…