Dicyclohexylcarbodiimide → 1,4,8-Trioxaspiro[4.5]decane-7,9-dione

HRID 231247노트

반응식

HRID 231247 반응식
[CH2:1]1[CH2:13][O:12][C:3]([CH2:8][C:9]([OH:11])=[O:10])([CH2:4][C:5](O)=[O:6])[O:2]1.C1(N=C=NC2CCCCC2)CCCCC1>O1CCCC1>[CH2:1]1[CH2:13][O:12][C:3]2([CH2:8][C:9](=[O:11])[O:10][C:5](=[O:6])[CH2:4]2)[O:2]1

참가 물질

4

반응물 2

HCID 10868DicyclohexylcarbodiimideHCID 133834462,2'-(1,3-Dioxolane-2,2-diyl)diacetic acid

생성물 1

HCID 133834501,4,8-Trioxaspiro[4.5]decane-7,9-dione수율 75%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of 3,3-(ethylenedioxy)glutaric acid (12.26 g, 64.50 mmole) in 300 ml of tetrahydrofuran maintained at 0° C. under nitrogen was added dropwise a solution of dicyclohexylcarbodiimide (13.60 g, 65.91 mmole) in 100 ml of tetrahydrofuran. The resulting suspension was stirred at room temperature overnight under nitrogen and the solvent was evaporated under vacuum. The residue was suspended in benzene, shaken thoroughly and filtered through silica gel packed in a column (10 cm long, SiO2, 60-200 mesh, benzene). The filtrate was evaporated under vacuum to provide the anhydride (8.268 g, 75% yield) as a white crystalline solid melting at about 111° C. to about 112° C.

후처리

  1. customthe solvent was evaporated under vacuum
  2. stirringshaken thoroughly
  3. filtrationfiltered through silica gel
  4. customThe filtrate was evaporated under vacuum

출처 및 근거

ORD 기록
ord-8b97b802c4064ba09ec68d8565a93d00
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04845229

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