Hydrochloric Acid → HCID 57795472, 화합물

HRID 1190066노트

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HRID 1190066 반응식
[CH3:1][N:2]1[C:6]2([CH2:15][CH2:14][C:9]3(OCC[O:10]3)[CH2:8][CH2:7]2)[CH2:5][N:4]([CH3:16])[C:3]1=[O:17].Cl>C1COCC1>[CH3:1][N:2]1[C:6]2([CH2:15][CH2:14][C:9](=[O:10])[CH2:8][CH2:7]2)[CH2:5][N:4]([CH3:16])[C:3]1=[O:17]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 57795511HCID 57795511, 화합물

생성물 1

HCID 57795472HCID 57795472, 화합물수율 66%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
50 °C

실험 절차

1,3-Dimethyl-9,12-dioxa-1,3-diaza-dispiro[4.2.4.2]tetradecan-2-one (3.16 g, 13.2 mmol) was dissolved in 66 mL of THF and a portion of 130 mL of 3N HCl aqueous solution was added. The resulting mixture was stirred at 50° C. for two days. THF was removed under vacuum then the remaining mixture was extracted with two portions of dichloromethane. The organic portions were combined, dried over anhydrous Na2SO4 and concentrated. The crude was purified by silica gel column chromatography using a gradient from 2% CH2Cl2:MeOH to 10% CH2Cl2:MeOH as eluent to afford 1,3-dimethyl-1,3-diaza-spiro[4.5]decane-2,8-dione (1.7 g, 66%).

후처리

  1. customTHF was removed under vacuum
  2. extractionthe remaining mixture was extracted with two portions of dichloromethane
  3. dry with materialdried over anhydrous Na2SO4
  4. concentrationconcentrated
  5. customThe crude was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-5af342be88a8454fb6994db6ac760df4
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08674118B2

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