Triethylamine → HCID 20403159, 화합물

HRID 2198474노트

반응식

HRID 2198474 반응식
[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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 108982-BromoethanolHCID 20403147HCID 20403147, 화합물

생성물 1

HCID 20403159HCID 20403159, 화합물수율 72%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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 is 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.

후처리

  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 is distilled under reduced pressure
  8. customto afford 28 g

출처 및 근거

ORD 기록
ord-7bd2a86e6f644581815fd0aee0f7710f
출처 데이터셋
uspto-grants-1982_11
특허 번호
US04357471

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