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Methylamine → rac-(1R,2R)-2-(methylamino)cyclohexan-1-ol

HRID 1720374
ノート
印刷プレビュー

反応式

HRID 1720374 の反応式
[CH:1]12[O:7][CH:2]1[CH2:3][CH2:4][CH2:5][CH2:6]2.[CH3:8][NH2:9].[OH-].[Na+]>>[CH3:8][NH:9][C@@H:1]1[CH2:6][CH2:5][CH2:4][CH2:3][C@H:2]1[OH:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 6329MethylamineHCID 9246Cyclohexene oxideHCID 14798Sodium Hydroxide

生成物 1

HCID 12847193rac-(1R,2R)-2-(methylamino)cyclohexan-1-ol

実験手順

Cyclohexene oxide (202 mL, 2 mol) was added dropwise to aqueous methyl amine (466 mL or 40% solution, 6 mol) over 70 minutes. After a further 90 minutes, the temperature of the reaction mixture was 48° C. and was reduced to 30° C. by cooling in a water bath. After a further 2 hours, the mixture had returned to room temperature. It was stirred overnight, and then refluxed for 3 h. The mixture was saturated with sodium hydroxide (cooled during addition), extracted several times with diethyl ether (total 500 mL), the diethyl ether layer dried over sodium sulphate overnight, and the diethyl ether removed on a rotary evaporator. The remaining diethyl ether and cyclohexene oxide were removed by partial vacuum distillation. Distillation under full vacuum yielded a colorless fraction boiling at 95° C., (±)-trans-2-(methylamino)cyclohexanol: 217 g (84%).

後処理

  1. customwas 48° C.
  2. customwas reduced to 30° C.
  3. temperatureby cooling in a water bath
  4. waitAfter a further 2 hours
  5. customhad returned to room temperature
  6. temperaturerefluxed for 3 h
  7. extractionextracted several times with diethyl ether (total 500 mL)
  8. dry with materialthe diethyl ether layer dried over sodium sulphate overnight
  9. customthe diethyl ether removed on a rotary evaporator
  10. customThe remaining diethyl ether and cyclohexene oxide were removed by partial vacuum distillation
  11. distillationDistillation under full vacuum

出典と根拠

ORDレコード
ord-25ac1325910a446687606c7b01c71d00
出典データセット
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05506257

反応ノート

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