Water → HCID 59860533、化合物

HRID 2421817ノート

反応式

HRID 2421817 の反応式
[CH3:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[CH2:4][CH2:5][CH:6]2O.C1(P([N:26]=[N+:27]=[N-:28])(C2C=CC=CC=2)=O)C=CC=CC=1.N12CCCN=C1CCCCC2.O>C1COCC1>[N:26]([CH:6]1[C:7]2[C:3](=[C:2]([CH3:1])[CH:10]=[CH:9][CH:8]=2)[CH2:4][CH2:5]1)=[N+:27]=[N-:28]

参加物

6

反応物 4

HCID 962WaterHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 199401P,P-Diphenylphosphinic azideHCID 109863964-methyl-2,3-dihydro-1H-inden-1-ol

生成物 1

HCID 59860533HCID 59860533、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

4.34 g (29.28 mmol) 4-methyl-indan-1-ol and 7.8 ml (35.14 mmol) diphenylphosphoryl azide are dissolved in dry THF at room temperature under argon. To this mixture is added slowly 5.0 ml (35.14 mmol) 1,8-diazabicyclo[5.4.0]undec-7-ene. The reaction is stirred for 6 h at room temperature (TLC monitoring). Then the mixture is poured into water and extracted three times with toluene. The organic layers are combined, dried over MgSO4 and concentrated in vacuo. Purification using silica gel chromatography (hexane/EtOAc 9:1) affords pure 1-azido-4-methyl-indane as light orange liquid.

後処理

  1. extractionextracted three times with toluene
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customPurification

出典と根拠

ORDレコード
ord-2f9902c6484e4d48a979168715ca2188
出典データセット
uspto-grants-2011_06
特許番号
US07960310B2

反応ノート

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