Triethylamine → HCID 86681323、化合物

HRID 1778905ノート

反応式

HRID 1778905 の反応式
Cl.[NH2:2][C:3]1([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.C(N(CC)CC)C.Br[CH2:22][CH2:23][O:24][CH2:25][CH2:26]Br>CN(C)C=O.C(OCC)(=O)C>[O:24]1[CH2:25][CH2:26][N:2]([C:3]2([C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]2)[CH2:22][CH2:23]1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 21521Bis(2-bromoethyl) etherHCID 11241228Ethyl 1-aminocyclohexane-1-carboxylate hydrochloride

生成物 1

HCID 86681323HCID 86681323、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Ethyl 1-aminocyclohexancarboxylate hydrogen chloride (5.800 g), triethylamine (13.62 mL) and 1-bromo-2-(2-bromoethoxy)ethane (4.21 mL) were stirred together in N,N-dimethylformamide (50 mL) at 95° C. overnight. The reaction mixture was diluted with ethyl acetate (150 mL), washed with water (100 mL) and brine (100 mL), dried over magnesium sulfate, filtered, and concentrated. Silica gel chromatography eluting with a gradient of 5% to 25% ethyl acetate/hexanes provided the title compound.

後処理

  1. washwashed with water (100 mL) and brine (100 mL)
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. washSilica gel chromatography eluting with a gradient of 5% to 25% ethyl acetate/hexanes

出典と根拠

ORDレコード
ord-8937afdeb1bd42099cd0d560abb315d5
出典データセット
uspto-grants-2016_02
特許番号
US09266877B2

反応ノート

読み込み中…