Ethanolamine → 2-((Triphenylmethyl)amino)ethanol

HRID 274414ノート

反応式

HRID 274414 の反応式
[CH2:1]([CH2:3][NH2:4])[OH:2].[C:5]1([C:11]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)Cl)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.Cl.C(CN)O>C(O)(C)C>[C:11]([NH:4][CH2:3][CH2:1][OH:2])([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)([C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

参加物

5

反応物 3

HCID 700EthanolamineHCID 6456Trityl chloride2 回HCID 74819Ethanolamine Hydrochloride

生成物 1

HCID 31256082-((Triphenylmethyl)amino)ethanol収率 99.4%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of ethanolamine (2-aminoethanol) (98%, 1.750 kg, 28.0 moles) in isopropanol (7.0 l) was stirred to yield a homogeneous solution. Thereto triphenylchloromethane (97%, 2.020 kg, 7.03 moles) was added slowly within 1 h at room temperature with stirring, whereat the temperature was not to exceed 30° C. After completed dissolution of triphenylchloromethane (whereat ethanolamine hydrochloride separated as a white precipitate) the reaction mixture was stirred for another hour and cooled to room temperature. The precipitate, which separated, was filtered off and the filtrate was poured into ice-cold water (8.0 l). The precipitate, which separated, was filtered off and dried in vacuo at a temperature not exceeding 50° C. Thus there were obtained 2.120 kg (98%) of the desired compound.

後処理

  1. customto yield a homogeneous solution
  2. stirringwith stirring, whereat the temperature
  3. customto exceed 30° C
  4. customseparated as a white precipitate) the reaction mixture
  5. stirringwas stirred for another hour
  6. customThe precipitate, which separated
  7. filtrationwas filtered off
  8. additionthe filtrate was poured into ice-cold water (8.0 l)
  9. customThe precipitate, which separated
  10. filtrationwas filtered off
  11. customdried in vacuo at a temperature not
  12. customexceeding 50° C

出典と根拠

ORDレコード
ord-2926bcce21ac4ce3b1750044ad8b047a
出典データセット
uspto-grants-1995_02
特許番号
US05389654

反応ノート

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