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Water → HCID 57971679, 화합물

HRID 2276985
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HRID 2276985 반응식
C[O:2][C:3](=[O:21])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][C:10](=[O:20])[NH:11][O:12][CH:13]([O:15][CH2:16][CH:17]([CH3:19])[CH3:18])[CH3:14].O.[OH-].[Li+]>C1COCC1>[CH2:16]([O:15][CH:13]([O:12][NH:11][C:10]([CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][C:3]([OH:21])=[O:2])=[O:20])[CH3:14])[CH:17]([CH3:19])[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 57971668HCID 57971668, 화합물

생성물 1

HCID 57971679HCID 57971679, 화합물수율 828.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

7-(1-Isobutoxy-ethoxycarbamoyl)-heptanoic acid methyl ester (36.6 g, 12.1 mmol, 1.0 eq) was stirred in THF (200 mL) and water (200 mL) in the presence of lithium hydroxide (8.68 g, 36.2 mmol, 3.0 eq) for 3 h at 50° C. THF was evaporated under vacuum and to the mixture water (100 mL) and ethyl acetate (200 mL) were added. The mixture was acidified cautiously to pH 3 by addition of 1N HCl. The organic phase was isolated and the aqueous layer re-extracted with ethyl acetate (150 mL). The organic phases were combined, dried (MgSO4), filtered and concentrated in vacuo. The product was obtained as a white solid (29.0 g, 83% yield), m/z 288 [M++H]+ and used in stage 4 without further purification.

후처리

  1. customTHF was evaporated under vacuum and to the mixture water (100 mL) and ethyl acetate (200 mL)
  2. additionwere added
  3. additionThe mixture was acidified cautiously to pH 3 by addition of 1N HCl
  4. customThe organic phase was isolated
  5. extractionthe aqueous layer re-extracted with ethyl acetate (150 mL)
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-a9827e44b5fd4876960bc8a7dcf6de4b
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09133104B2

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