Hydrochloric Acid → 2-(Morpholin-4-yl)acetic acid hydrochloride
反応式
[O:1]1[CH2:6][CH2:5][N:4]([CH2:7][C:8]([O:10]C(C)(C)C)=[O:9])[CH2:3][CH2:2]1.[ClH:15]>O1CCOCC1.C(OCC)C>[ClH:15].[O:1]1[CH2:6][CH2:5][N:4]([CH2:7][C:8]([OH:10])=[O:9])[CH2:3][CH2:2]1参加物
5
実験手順
Tert-butyl 2-morpholinoacetate (11 g, 54.7 mmol) was stirred with HCl, 4M in dioxane (54 mL), giving a white precipitate (a mild exotherm was observed) which slowly dissolved with stirring at room temperature. Ten minutes after complete dissolution, the mixture solidified. Then the mixture was warmed to 60° C. and the thick suspension was stirred vigorously overnight. The mixture was then cooled to room temperature, diluted with diethyl ether (60 mL) and filtered to collect the title compound (8 g, 80%) as a white solid. 1H NMR (CD3OD, 400 MHz): δ (ppm) 4.13 (s, 2H), 3.94 (brm, 4H), 3.41 (brm, 4H).
後処理
- customgiving a white precipitate (a mild exotherm
- dissolutionslowly dissolved
- dissolutionTen minutes after complete dissolution
- temperatureThen the mixture was warmed to 60° C.
- stirringthe thick suspension was stirred vigorously overnight
- temperatureThe mixture was then cooled to room temperature
- filtrationfiltered
- customto collect the title compound (8 g, 80%) as a white solid
出典と根拠
- ORDレコード
- ord-39f24acd253746de84cead7c8fabe78f
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09441012B2
反応ノート
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