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1-Bromopropane → (6-Methyl-1,3-benzodioxol-5-yl)butan-1-ol

HRID 1195316
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반응식

HRID 1195316 반응식
[CH3:1][C:2]1[C:7]([CH:8]=[O:9])=[CH:6][C:5]2[O:10][CH2:11][O:12][C:4]=2[CH:3]=1.[Mg].Br[CH2:15][CH2:16][CH3:17].[Cl-].[NH4+]>O1CCCC1>[CH3:1][C:2]1[C:7]([CH:8]([OH:9])[CH2:15][CH2:16][CH3:17])=[CH:6][C:5]2[O:10][CH2:11][O:12][C:4]=2[CH:3]=1
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참가 물질

6

반응물 4

HCID 78401-BromopropaneHCID 25517Ammonium ChlorideHCID 31462426-Methyl-2H-1,3-benzodioxole-5-carbaldehydeHCID 5462224Magnesium

생성물 1

HCID 67784687(6-Methyl-1,3-benzodioxol-5-yl)butan-1-ol수율 88.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매
2회

실험 절차

A solution of 5.0 g of (6-methyl-1,3-benzodioxol-5-yl)-carboxaldehyde in 20 ml of tetrahydrofuran was dropwise added at a room temperature to a Grignard reagent prepared from 0.86 g of magnesium ribbon, 10 ml of tetrahydrofuran and 4.4 g of 1-bromopropane. The obtained mixture was stirred at a room temperature for one hour, followed by the addition of a saturated aqueous solution of ammonium chloride The obtained mixture was extracted with ether. The organic layer was washed with an aqueous solution of common salt, dried over magnesium sulfate and distilled to remove the solvent. 5.6 g of (6-methyl-1,3-benzodioxol-5-yl)-butan-1-ol was obtained.

후처리

  1. extractionwas extracted with ether
  2. washThe organic layer was washed with an aqueous solution of common salt
  3. dry with materialdried over magnesium sulfate
  4. distillationdistilled
  5. customto remove the solvent

출처 및 근거

ORD 기록
ord-59d1036511d445a7b7d91d6e227d0509
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05110956

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