Sodium Iodide → HCID 57608436、化合物

HRID 517132ノート

反応式

HRID 517132 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][CH:9]([OH:12])[CH2:10]Cl)[CH:5]=[CH:6][CH:7]=1.[N-:13]=[N+:14]=[N-:15].[Na+].[Na+].[I-]>CN(C=O)C.CCOCC>[N:13]([CH2:10][CH:9]([OH:12])[CH2:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Br:1])[CH:3]=1)=[N+:14]=[N-:15]

参加物

6

反応物 3

HCID 5238Sodium IodideHCID 33557Sodium AzideHCID 576084881-(3-Bromophenyl)-3-chloropropan-2-ol

生成物 1

HCID 57608436HCID 57608436、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
75 °C

実験手順

To a solution of 1-(3-bromophenyl)-3-chloropropan-2-ol (8.49 g, 34.0 mmol) in anhydrous DMF (100 mL) under N2 was added NaN3 (11.05 g, 170.0 mmol) and NaI (cat., 0.75 g, 5.0 mmol). The mixture was heated at 75° C. overnight. After cooling to room temperature, the mixture was diluted with ether and washed with water and brine. The solution was dried over Na2SO4 and concentrated under reduced pressure. The product was dried in a vacuum oven at 40° C. for 2 h to give 1-azido-3-(3-bromophenyl)propan-2-ol as a yellow oil which was used without purification. Yield (8.6 g, 98% crude).

後処理

  1. temperatureAfter cooling to room temperature
  2. washwashed with water and brine
  3. dry with materialThe solution was dried over Na2SO4
  4. concentrationconcentrated under reduced pressure
  5. customThe product was dried in a vacuum oven at 40° C. for 2 h

出典と根拠

ORDレコード
ord-aad59ba0cb494603a055712f36fd1afb
出典データセット
uspto-grants-2015_08
特許番号
US09115056B2

反応ノート

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