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

HRID 11836ノート

反応式

HRID 11836 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d2bf217eddca4257ae51da4d5cb2c928
出典データセット
uspto-grants-2006_08
特許番号
US07098215B2

反応ノート

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