Water → HCID 59860533, 화합물

HRID 2421817노트

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HRID 2421817 반응식
[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]

참가 물질

6

반응물 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

생성물 1

HCID 59860533HCID 59860533, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-2f9902c6484e4d48a979168715ca2188
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07960310B2

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