Water → HCID 178484843, 화합물

HRID 630374

반응식

HRID 630374 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([NH:14][C:15](=O)OC(C)(C)C)[CH2:10][CH2:9]1.O.[OH-].[Na+]>O1CCCC1.C(Cl)(Cl)Cl>[CH3:15][NH:14][C@H:11]1[CH2:12][CH2:13][C@H:8]([OH:7])[CH2:9][CH2:10]1

참가 물질

7

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 178418329HCID 178418329, 화합물2회

생성물 1

HCID 178484843HCID 178484843, 화합물수율 89%

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of lithium aluminium hydride (9 g, 0.23 mol) in tetrahydrofuran (425 mL) was added slowly tert-butyl (trans-4-hydroxycyclohexyl)carbamate (intermediate 1, 10 g, 0.046 mol). The mixture was refluxed overnight. Once the mixture was cooled to room temperature, 9 ml of water, 9 ml of 4N NaOH solution and 18 ml of water were carefully and successively dropped. The organic solvent was removed under reduced pressure and the crude obtained was dissolved with chloroform and dried over magnesium sulphate. The filtrate was evaporated to dryness and co evaporated with hexane to give the title compound as a white solid (89%). This intermediate is also described in JMC, 1987, 30(2), p 313.

후처리

  1. temperatureThe mixture was refluxed overnight
  2. additionsuccessively dropped
  3. customThe organic solvent was removed under reduced pressure
  4. customthe crude obtained
  5. dry with materialdried over magnesium sulphate
  6. customThe filtrate was evaporated to dryness and co
  7. customevaporated with hexane

출처 및 근거

ORD 기록
ord-6778815796a845dda765468e30c93e3b
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315463B2

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