Sodium Hydroxide → HCID 67284959, 화합물

HRID 1618792노트

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HRID 1618792 반응식
[CH3:1][C:2]1([CH3:23])[O:22][CH2:21][C:5]2([C:13]3[C:8](=[CH:9][C:10]([N:14]4[CH2:19][CH2:18][O:17][CH2:16][CH2:15]4)=[CH:11][CH:12]=3)[NH:7][C:6]2=O)[CH2:4][O:3]1.[H-].COCCO[Al+]OCCOC.[Na+].[H-].[OH-].[Na+]>C1(C)C=CC=CC=1>[CH3:1][C:2]1([CH3:23])[O:3][CH2:4][C:5]2([C:13]3[C:8](=[CH:9][C:10]([N:14]4[CH2:15][CH2:16][O:17][CH2:18][CH2:19]4)=[CH:11][CH:12]=3)[NH:7][CH2:6]2)[CH2:21][O:22]1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 21584525Sodium bis(2-methoxyethoxy)aluminiumhydrideHCID 67284582HCID 67284582, 화합물

생성물 1

HCID 67284959HCID 67284959, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
80 °C

실험 절차

To a solution of 2,2-dimethyl-6′-morpholinospiro[[1,3]dioxane-5,3′-indolin]-2′-one (0.11 g, 0.35 mmol) in toluene (14 mL) was added sodium bis(2-methoxyethoxy)aluminium hydride (60% in toluene, 0.53 mL, 1.74 mmol). After stirring at 80° C. for 40 min, the solution was poured into a mixture of ice and 2N NaOH. The product was extracted with DCM and the combined organic extracts were dried over MgSO4, filtered and evaporated in vacuo. Purification by column chromatography (eluting with a gradient of 5-60% EtOAc in hexanes) gave 2,2-dimethyl-6′-morpholinospiro[[1,3]dioxane-5,3′-indoline] as a white solid. Mass Spectrum (ESI) m/e=305.2 (M+1).

후처리

  1. extractionThe product was extracted with DCM
  2. dry with materialthe combined organic extracts were dried over MgSO4
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. customPurification by column chromatography (
  6. washeluting with a gradient of 5-60% EtOAc in hexanes)

출처 및 근거

ORD 기록
ord-d26d51b5318647488b097138cc43d970
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765940B2

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