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Lithium Hydroxide → HCID 178443426, 화합물

HRID 1681544
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HRID 1681544 반응식
[CH2:1]([O:11][C:12]1[CH:30]=[CH:29][C:15]([C:16]([C:18]2[CH:19]=[C:20]([CH:26]=[CH:27][CH:28]=2)[C:21]([O:23]CC)=[O:22])=[O:17])=[CH:14][C:13]=1[CH2:31][C:32]1[NH:36][N:35]=[N:34][N:33]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[OH-].[Li+]>CC(C)=O.O>[CH2:1]([O:11][C:12]1[CH:30]=[CH:29][C:15]([C:16]([C:18]2[CH:19]=[C:20]([CH:26]=[CH:27][CH:28]=2)[C:21]([OH:23])=[O:22])=[O:17])=[CH:14][C:13]=1[CH2:31][C:32]1[NH:36][N:35]=[N:34][N:33]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 178443427HCID 178443427, 화합물

생성물 1

HCID 178443426HCID 178443426, 화합물수율 8.6%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

A mixture of 580 mg of the product from Example 2 and 280 mg of lithium hydroxide in 10 ml of acetone and 1 ml of water were stirred for 6 hours. The mixture was concentrated in vacuo and the resulting residue was partitioned between diethyl ether and water. The layers were separated and the aqueous layer was extracted with diethyl ether. The aqueous layer was acidified with 1N hydrochloric acid and extracted with ethyl acetate. The ethyl acetate extract was dried over magnesium sulfate and concentrated to dryness. The residue was crystallized from hexane/ethyl acetate to provide 47 mg of the title product, m.p. 147°-150° C.

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe resulting residue was partitioned between diethyl ether and water
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with diethyl ether
  5. extractionextracted with ethyl acetate
  6. extractionThe ethyl acetate extract
  7. dry with materialwas dried over magnesium sulfate
  8. concentrationconcentrated to dryness
  9. customThe residue was crystallized from hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-905ada7383d24b5eb58df71a16257f65
출처 데이터셋
uspto-grants-1992_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05171882

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