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Sodium Hydroxide → HCID 25183514, 화합물

HRID 1925744
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HRID 1925744 반응식
[CH2:1]1[C:9]2[C:4](=[CH:5][C:6]([S:10]([NH:13][C:14]3[CH:18]=[CH:17][S:16][C:15]=3[C:19]([O:21]C)=[O:20])(=[O:12])=[O:11])=[CH:7][CH:8]=2)[CH2:3][CH2:2]1.[OH-].[Na+]>O1CCCC1.CO>[CH2:1]1[C:9]2[C:4](=[CH:5][C:6]([S:10]([NH:13][C:14]3[CH:18]=[CH:17][S:16][C:15]=3[C:19]([OH:21])=[O:20])(=[O:11])=[O:12])=[CH:7][CH:8]=2)[CH2:3][CH2:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 8823202HCID 8823202, 화합물

생성물 1

HCID 25183514HCID 25183514, 화합물수율 100.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

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온도
80 °C

실험 절차

To a solution of 125 (0.30 g; 0.89 mmol) in tetrahydrofuran (20 mL) and methanol (7 mL) was added aqueous sodium hydroxide (20 mL; 2N) and then heated at 80° C. for 16 hours. The reaction mixture was allowed to cool to room temperature and then extracted with diethyl ether (20 mL). The aqueous layer was separated and acidified with aqueous hydrochloric acid (15 mL; 2N) then extracted with ethyl acetate (2×20 mL). The combined organic phases were dried over magnesium sulfate, filtered, and concentrated under reduced pressure to yield the title product as an off-white solid (0.29 g).

후처리

  1. temperatureto cool to room temperature
  2. extractionextracted with diethyl ether (20 mL)
  3. customThe aqueous layer was separated
  4. extractionthen extracted with ethyl acetate (2×20 mL)
  5. dry with materialThe combined organic phases were dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-566b62d6d89b4df58f60af43eadb1342
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08178699B2

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