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Lithium hydroxide, monohydrate → HCID 21251123, 화합물

HRID 1275642
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HRID 1275642 반응식
C[O:2][C:3]([C:5]1[C:9]([N:10]([S:18]([C:21]2[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[CH:23][CH:22]=2)(=[O:20])=[O:19])[CH2:11][C:12]2[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=2)=[C:8]([Br:29])[S:7][CH:6]=1)=[O:4].O.[OH-].[Li+]>C1COCC1.CO>[Br:29][C:8]1[S:7][CH:6]=[C:5]([C:3]([OH:4])=[O:2])[C:9]=1[N:10]([S:18]([C:21]1[CH:22]=[CH:23][C:24]([O:27][CH3:28])=[CH:25][CH:26]=1)(=[O:19])=[O:20])[CH2:11][C:12]1[CH:13]=[N:14][CH:15]=[CH:16][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 9870466HCID 9870466, 화합물

생성물 1

HCID 21251123HCID 21251123, 화합물수율 100%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

실험 절차

To a solution of 0.40 g (0.860 mmol) of the product of Example 24 in 9.0 mL of THF-MeOH (1:1) was added 0.072 g (1.72 mmol) of lithium hydroxide monohydrate. The reaction mix was heated to reflux for 18 h and then concentrated in vacuo. The residue was was washed with THF and filtered. The filtrate was concentrated in vacuo to provide 0.388 g (100%) of the desired product as a white foam. Electrospray Mass Spec: 483 (M+H).

후처리

  1. additionThe reaction mix
  2. temperaturewas heated
  3. temperatureto reflux for 18 h
  4. concentrationconcentrated in vacuo
  5. washThe residue was was washed with THF
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-713b0e5b14444848979ffbd311b63bcf
출처 데이터셋
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06162821

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