Water → HCID 178484843、化合物

HRID 630374

反応式

HRID 630374 の反応式
[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

参加物

7

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 178418329HCID 178418329、化合物2 回

生成物 1

HCID 178484843HCID 178484843、化合物収率 89%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6778815796a845dda765468e30c93e3b
出典データセット
uspto-grants-2016_04
特許番号
US09315463B2

関連ノート

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