Triethylamine → HCID 20403159、化合物

HRID 1758813ノート

反応式

HRID 1758813 の反応式
[CH2:1]1[C:6]2([CH2:11][CH2:10][CH2:9][CH:8]=[CH:7]2)[CH2:5][CH2:4][CH2:3][NH:2]1.Br[CH2:13][CH2:14][OH:15].C(N(CC)CC)C>C1(C)C=CC=CC=1>[OH:15][CH2:14][CH2:13][CH:1]1[C:6]2([CH2:11][CH2:10][CH2:9][CH:8]=[CH:7]2)[CH2:5][CH2:4][CH2:3][NH:2]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 108982-BromoethanolHCID 20403147HCID 20403147、化合物

生成物 1

HCID 20403159HCID 20403159、化合物収率 72%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 2-azaspiro-[5.5]-undec-7-ene (30.2 g.; 0.20 mole), 2-bromoethanol (25 g.; 0.20 mole) and triethylamine (20.2 g.) in toluene (250 ml.) is heated under reflux for 5 hours. The solution is cooled, filtered to remove triethylamine hydrobromide and the filtrate concentrated under reduced pressure. The residual liquid was distilled under reduced pressure to afford 28 g. (72% yield) of 2-hydroxyethyl-2-azaspiro-[5.5]-undec-7-ene, b.p. 90°-91° C./0.45 mm.

後処理

  1. temperatureis heated
  2. temperatureunder reflux for 5 hours
  3. temperatureThe solution is cooled
  4. filtrationfiltered
  5. customto remove triethylamine hydrobromide
  6. concentrationthe filtrate concentrated under reduced pressure
  7. distillationThe residual liquid was distilled under reduced pressure
  8. customto afford 28 g

出典と根拠

ORDレコード
ord-6c6d029ad08e4cf49dd28c13c5d9522a
出典データセット
uspto-grants-1983_02
特許番号
US04374991

反応ノート

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