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Hydrochloric Acid → HCID 86200540、化合物

HRID 718154
ノート
印刷プレビュー

反応式

HRID 718154 の反応式
[CH3:1][O:2][CH2:3][CH2:4][C:5]#[N:6].[ClH:7].[CH2:8]([OH:10])[CH3:9]>>[ClH:7].[CH3:1][O:2][CH2:3][CH2:4][C:5](=[NH:6])[O:10][CH2:8][CH3:9]
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 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 61032Propanenitrile, 3-methoxy-

生成物 1

HCID 86200540HCID 86200540、化合物収率 63%

実験手順

3-Methoxypropanenitrile (5.0 g, 58.8 mmol) was dissolved in anhydrous ethanol (50 mL) under an atmosphere of Ar. The solution was cooled to 0° C., saturated with HCl gas, stirred for 6 h, allowed to warm to RT, and stirred for 6 h. The solvent was removed in vacuo. The residue was slurried with hexanes (50 mL) and sonicated for 10 min. The solids were allowed to settle and the solvent was removed by decantation. This was repeated (3×). The solid was collected and dried under high vacuum for 5 h to afford ethyl 3-methoxypropanimidate hydrochloride (6.2 g, 63%) as a white solid. 1H NMR (400 MHz, DMSO-d6): δ 12.03 (br s, 1H), 11.22 (br s, 1H), 4.42 (q, J=7.0 Hz, 2H), 3.60 (t, J=5.9 Hz, 2H), 3.23 (s, 3H), 2.87 (t, J=5.9 Hz, 2H), 1.33 (t, J=7.0 Hz, 3H).

後処理

このページの内容参加物実験手順後処理出典と根拠反応ノート
  1. stirringstirred for 6 h
  2. customThe solvent was removed in vacuo
  3. customsonicated for 10 min
  4. customthe solvent was removed by decantation
  5. customThe solid was collected
  6. customdried under high vacuum for 5 h

出典と根拠

ORDレコード
ord-087009a2667c42a281c7f3050fed48bb
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09193719B2

反応ノート

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