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Sodium Hydroxide → HCID 19047814, 화합물

HRID 1198068
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HRID 1198068 반응식
C([O:3][C:4]([C:6]1[N:7]([S:15]([C:18]2[CH:23]=[CH:22][C:21]([CH3:24])=[CH:20][CH:19]=2)(=[O:17])=[O:16])[C:8]2[C:13]([CH:14]=1)=[CH:12][CH:11]=[CH:10][CH:9]=2)=O)C.[OH-].[Na+]>C1(C)C=CC=CC=1.C1COCC1>[OH:3][CH2:4][C:6]1[N:7]([S:15]([C:18]2[CH:19]=[CH:20][C:21]([CH3:24])=[CH:22][CH:23]=2)(=[O:17])=[O:16])[C:8]2[C:13]([CH:14]=1)=[CH:12][CH:11]=[CH:10][CH:9]=2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 14783456Nod-IN-1

생성물 1

HCID 19047814HCID 19047814, 화합물수율 99.1%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8028Tetrahydrofuran용매2회

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온도
5 °C

실험 절차

To stirred solution of Red-A1 (sodium dihydro-bis(2-methoxyethoxy)aluminate ≈70% in toluene) (30 mL) in dry THF (100 mL) cooled at 5° C. and under nitrogen was added dropwise and at this temperature a solution of compound of step 1 (26,8 g, 78 mmol) in dry THF (75 mL). After stirring one hour at 5° C. and then one hour at room temperature the mixture was cooled at 10° C. and treated dropwise with 2N NaOH, to effect hydrolysis of the intermediate complex. The organic phase was separated and the solvent in vacuo evaporated. The residue was solved in ethyl ether, the solution washed with water, dried over MgSO4 and evaporated to give the required alcohol (23.3 g, 98%) as a yellow oil; IR (film) 3500, 1597 cm-1.

후처리

  1. temperatureone hour at room temperature the mixture was cooled at 10° C.
  2. customhydrolysis of the intermediate complex
  3. customThe organic phase was separated
  4. customthe solvent in vacuo evaporated
  5. washthe solution washed with water
  6. dry with materialdried over MgSO4
  7. customevaporated

출처 및 근거

ORD 기록
ord-2571411b9fd44a13813a11a2d77a544e
출처 데이터셋
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05278316

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