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Hydrochloric Acid → HCID 86200540, 화합물

HRID 718154
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HRID 718154 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

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

생성물 1

HCID 86200540HCID 86200540, 화합물수율 63%

실험 절차

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).

후처리

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트
  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

출처 및 근거

ORD 기록
ord-087009a2667c42a281c7f3050fed48bb
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09193719B2

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