Water → 4-(Diphenylmethoxy)-1-piperidineethanol

HRID 443799ノート

反応式

HRID 443799 の反応式
[C:1]1([CH:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[O:8][CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:21]1[O:23][CH2:22]1.O>CO>[OH:23][CH2:22][CH2:21][N:12]1[CH2:13][CH2:14][CH:9]([O:8][CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH2:10][CH2:11]1

参加物

5

反応物 3

HCID 962WaterHCID 6354Ethylene OxideHCID 30175844-Benzhydryloxypiperidine

生成物 1

HCID 229894124-(Diphenylmethoxy)-1-piperidineethanol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The starting material is obtained as follows. The solution of 13.35 g of 4-diphenylmethoxypiperidine in 40 ml of methanol, containing 3.52 g of ethylene oxide and 0.9 ml of water, is stirred and heated in an oil bath at 42°-44° for 4 hours. The bath temperature is raised to 50° and heating and stirring are continued for an additional 3 hours. The solution is then evaporated and the residue taken up in 1 N hydrochloric acid and washed with diethyl ether. The aqueous solution is made basic with 50% aqueous sodium hydroxide and repeatedly extracted with diethyl ether. The extract is washed with brine, dried and evaporated to give the 1-(2-hydroxyethyl)-4-diphenylmethoxypiperidine, melting at 83°-85° after recrystallization from cyclohexane.

後処理

  1. customThe starting material is obtained
  2. temperatureheated in an oil bath at 42°-44° for 4 hours
  3. temperatureThe bath temperature is raised to 50°
  4. temperatureheating
  5. stirringstirring
  6. customThe solution is then evaporated
  7. washwashed with diethyl ether
  8. extractionrepeatedly extracted with diethyl ether
  9. washThe extract is washed with brine
  10. customdried
  11. customevaporated

出典と根拠

ORDレコード
ord-5f3588da20924c4e8d4ec09107d900ff
出典データセット
uspto-grants-1981_04
特許番号
US04261990

反応ノート

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