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Methylamine → 11-(Methylamino)undecan-1-ol

HRID 1052938
ノート
印刷プレビュー

反応式

HRID 1052938 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][OH:13].[CH3:14][NH2:15]>C(O)C>[CH3:14][NH:15][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][OH:13]
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 2

HCID 6329MethylamineHCID 7416311-Bromo-1-undecanol

生成物 1

HCID 1976727411-(Methylamino)undecan-1-ol収率 67%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 11-bromoundecanol (25.12 g, 0.10 mol) and methylamine (41% in water, 127 ml, 1.50 mol) in ethanol (50 ml) was heated for 7 h to 70° C. and stirred for a further 16 h at ambient temperature. The solvent was distilled off. After cooling the white solid was dissolved in caustic soda (2N, 200 ml) and diethyl ether (300 ml). The phases were separated and the aqueous phase was extracted with diethyl ether (2×100 ml). The combined organic phases were dried over Na2SO4, filtered and concentrated on the rotary evaporator. The crude product was recrystallized from diethyl ether. 13.23 g (65.7 mmol, 67% yield) of a while solid (melting point: 58° C.) was obtained.

後処理

  1. distillationThe solvent was distilled off
  2. temperatureAfter cooling the white solid
  3. dissolutionwas dissolved in caustic soda (2N, 200 ml)
  4. customThe phases were separated
  5. extractionthe aqueous phase was extracted with diethyl ether (2×100 ml)
  6. dry with materialThe combined organic phases were dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated on the rotary evaporator
  9. customThe crude product was recrystallized from diethyl ether

出典と根拠

ORDレコード
ord-37f1f55fa8c34964ae58c3100ebe2b4d
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09393181B2

反応ノート

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