Water → HCID 21070649、化合物

HRID 1435345ノート

反応式

HRID 1435345 の反応式
[CH3:1][S:2]([N:5]1[CH2:11][CH2:10][CH:9]2[CH:7]([O:8]2)[CH2:6]1)(=[O:4])=[O:3].[N-:12]=[N+:13]=[N-:14].[Na+].O>CN(C)C=O>[N:12]([CH:9]1[CH2:10][CH2:11][N:5]([S:2]([CH3:1])(=[O:4])=[O:3])[CH2:6][CH:7]1[OH:8])=[N+:13]=[N-:14]

参加物

5

反応物 3

HCID 962WaterHCID 33557Sodium AzideHCID 13042966HCID 13042966、化合物

生成物 1

HCID 21070649HCID 21070649、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

To a stirred solution of rac-3-methanesulfonyl-7-oxa-3-aza-bicyclo[4.1.0]heptane (0.92 g, 5.19 mmol, Example 303) in dimethylformamide (20 mL), sodium azide (550 mg, 8.46 mmol) was added and the mixture was stirred at 80° C. for 6 hours. The mixture was cooled and poured into water and extracted with ethyl acetate (3×10 mL). The extracts were combined, washed with water, brine and dried with MgSO4. The solvent was removed to give the desired product as colorless oil. 304 mg, 30.4%. The compound was used directly for the next step.

後処理

  1. temperatureThe mixture was cooled
  2. extractionextracted with ethyl acetate (3×10 mL)
  3. washwashed with water, brine
  4. dry with materialdried with MgSO4
  5. customThe solvent was removed

出典と根拠

ORDレコード
ord-217106aa8c144b408b45fceb683f95fe
出典データセット
uspto-grants-2009_11
特許番号
US07615634B2

反応ノート

読み込み中…