Sodium Azide → 3-Azido-1-benzhydrylazetidine

HRID 323604

反応式

HRID 323604 の反応式
[CH:1]([N:14]1[CH2:17][CH:16](OS(C2C=CC(C)=CC=2)(=O)=O)[CH2:15]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N-:29]=[N+:30]=[N-:31].[Na+]>CN(C=O)C>[N:29]([CH:16]1[CH2:17][N:14]([CH:1]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH2:15]1)=[N+:30]=[N-:31]

参加物

4

反応物 2

HCID 33557Sodium AzideHCID 155126511-Benzhydrylazetidin-3-yl 4-methylbenzenesulfonate

生成物 1

HCID 155126523-Azido-1-benzhydrylazetidine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 9 (11.5 g, 31.8 mmol) and sodium azide (4.12 g, 64 mmol) in 250 ml of DMF was heated to 70° C. for 24 hours. After cooling to room temperature the solvent was removed in vacuo and the residue partitioned between chloroform and water. The organics were dried over MgSO4, filtered and the solvent removed in vacuo. The crude product was purified by chromatography on silica gel (8:1 hexane: ethyl acetate) afforded the title compound.

後処理

  1. customwas removed in vacuo
  2. customthe residue partitioned between chloroform and water
  3. dry with materialThe organics were dried over MgSO4
  4. filtrationfiltered
  5. customthe solvent removed in vacuo
  6. customThe crude product was purified by chromatography on silica gel (8:1 hexane: ethyl acetate)

出典と根拠

ORDレコード
ord-b1217393730944209c1603dc36d443ea
出典データセット
uspto-grants-2001_04
特許番号
US06214832B1

関連ノート

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