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Water → 8-(2-Propenyloxy)-1,4-dioxaspiro[4.5]decane

HRID 2392738
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HRID 2392738 반응식
[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([OH:11])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.[H-].[Na+].[CH2:14](Br)[CH:15]=[CH2:16].O>CN(C)C=O>[CH2:16]([O:11][CH:8]1[CH2:9][CH2:10][C:5]2([O:4][CH2:3][CH2:2][O:1]2)[CH2:6][CH2:7]1)[CH:15]=[CH2:14]
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참가 물질

6

반응물 4

HCID 962WaterHCID 7841Allyl bromideHCID 24758Sodium hydrideHCID 5673521,4-Dioxaspiro(4.5)decan-8-ol

생성물 1

HCID 189805108-(2-Propenyloxy)-1,4-dioxaspiro[4.5]decane수율 81%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
20 °C

실험 절차

23.7 g (150 mmole) 1,4-dioxa-spiro[4.5]decan-8-ol were dissolved in 120 ml absolute dimethylformamide under a nitrogen atmosphere. After adding 7.9 g of 50% sodium hydride in mineral oil (165 mmole), the mixture was stirred for 1 hour at 20° C. After adding 14.3 ml allyl bromide (165 mmole), the mixture was heated to 70° C. and stirred for 1 hour. Thereafter it was treated with 160 ml water and was extracted at 10° C.-15° C., three times with ether, once with water and once with saturated sodium chloride solution. After removing the solvent by distillation, 24 g of crude product (81% theoretical) were obtained.

후처리

  1. temperaturethe mixture was heated to 70° C.
  2. stirringstirred for 1 hour
  3. extractionwas extracted at 10° C.-15° C.
  4. customAfter removing the solvent
  5. distillationby distillation

출처 및 근거

ORD 기록
ord-5fc74dfa42f948c5875825b728ac3ebc
출처 데이터셋
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05801201

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