Water → HCID 178484806, 화합물

HRID 2057241노트

반응식

HRID 2057241 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].C[O:8][C:9]([C@H:11]1[CH2:16][CH2:15][C@H:14]([NH:17][C:18](OC(C)(C)C)=O)[CH2:13][CH2:12]1)=O.O>C1COCC1>[CH3:18][NH:17][C@H:14]1[CH2:15][CH2:16][C@H:11]([CH2:9][OH:8])[CH2:12][CH2:13]1

참가 물질

5

반응물 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 178501239HCID 178501239, 화합물

생성물 1

HCID 178484806HCID 178484806, 화합물수율 100.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

반응 조건

온도
0 °C

실험 절차

A solution of 1.52 g (40 mmol) LAH in 7 ml THF was refluxed and treated for 2.5 h with a solution of 5.15 g (20 mmol) of trans-4-tert-butoxycarbonylamino-cyclohexanecarboxylic acid methyl ester in 35 ml THF. The reaction was heated for 15 h, cooled (0° C.) and hydrolyzed with 10 ml water. The mixture was diluted with THF, dried over Na2SO4, filtered and evaporated. The residue was dissolved in CH2Cl2, dried over Na2SO4, filtered and evaporated to yield 2.89 g (100%) of trans-(4-Methylamino-cyclohexyl)-methanol, mp: 87-88° C.; MS: 143 (M).

후처리

  1. temperatureThe reaction was heated for 15 h
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. customevaporated
  5. dissolutionThe residue was dissolved in CH2Cl2
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-b951b844a1b04c57a216d08e275ba650
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07335687B2

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