Benzylamine → HCID 69256693、化合物

HRID 1793339ノート

反応式

HRID 1793339 の反応式
CS(O[CH2:6][C@H:7]1[O:16][C:11]2=[N:12][CH:13]=[CH:14][CH:15]=[C:10]2[O:9][CH2:8]1)(=O)=O.[CH2:17]([NH2:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C([O-])(O)=O.[Na+]>O1CCOCC1>[C:18]1([CH2:17][NH:24][CH2:6][C@@H:7]2[O:16][C:11]3=[N:12][CH:13]=[CH:14][CH:15]=[C:10]3[O:9][CH2:8]2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

5

反応物 3

HCID 7504BenzylamineHCID 516892Sodium BicarbonateHCID 131725870HCID 131725870、化合物

生成物 1

HCID 69256693HCID 69256693、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of intermediate (3) (0.041 mol), benzylamine (0.041 mol) and NaHCO3 (0.11 mol) in dioxane (100 ml) was stirred and refluxed for 48 hours. The solvent was evaporated. The residue was taken up in water and DCM. The separated organic layer was dried, filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5). The desired fractions were collected, the solvent was evaporated, yielding (S)-2,3-dihydro-N-(phenylmethyl)-[1,4]dioxino[2,3-b]pyridine-3-methanamine (intermediate 55).

後処理

  1. temperaturerefluxed for 48 hours
  2. customThe solvent was evaporated
  3. customThe separated organic layer was dried
  4. filtrationfiltered
  5. customthe solvent was evaporated
  6. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
  7. customThe desired fractions were collected
  8. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-5e097a300e7d4722996dea0fb55be713
出典データセット
uspto-grants-2006_07
特許番号
US07081453B2

反応ノート

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