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Sodium Hydroxide → 5-Methoxy-6-(trifluoromethyl)indoline

HRID 427729
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HRID 427729 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[C:12]([F:15])([F:14])[F:13])[NH:8][CH:7]=[CH:6]2.C([BH3-])#N.[Na+].[OH-].[Na+]>C(O)(=O)C.O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[C:12]([F:15])([F:13])[F:14])[NH:8][CH2:7][CH2:6]2
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참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 5003444Sodium cyanoborohydrideHCID 108225525-Methoxy-6-(trifluoromethyl)-1H-indole

생성물 1

HCID 112067135-Methoxy-6-(trifluoromethyl)indoline수율 99%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

5 The indole (D8) (67.63 g, 0.315 mol) in glacial acetic acid (500 ml) was treated with sodium cyanoborohydride (40 g, 0.637 mol) at room temperature with stirring. After 3 h at room temperature the reaction mixture was diluted with water (500 ml) and basified with 40% aqueous NaOH with cooling. The mixture was then extracted with dichloromethane (3×500 ml) and the combined extracts were dried (Na2SO4) and evaporated to give the title compound (67.73 g, 99%) as an off-white solid.

후처리

  1. temperaturewith cooling
  2. extractionThe mixture was then extracted with dichloromethane (3×500 ml)
  3. dry with materialthe combined extracts were dried (Na2SO4)
  4. customevaporated

출처 및 근거

ORD 기록
ord-359c6b5f5b7c4063a34ec072aca6c3cf
출처 데이터셋
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06313145B1

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