Methanol → HCID 59775598, 화합물

HRID 557465노트

반응식

HRID 557465 반응식
[NH2:1][CH:2]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([I:13])[CH:8]=1)[CH2:3][C:4]([OH:6])=[O:5].S(Cl)(Cl)=O.[CH3:18]O>>[CH3:18][O:5][C:4](=[O:6])[CH2:3][CH:2]([NH2:1])[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([I:13])[CH:8]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 27723423-Amino-3-(3-iodophenyl)propanoic acid

생성물 1

HCID 59775598HCID 59775598, 화합물수율 95%

실험 절차

To a suspension of (±)-3-Amino-3-(3-iodo-phenyl)-propionic acid (3.1 g, 10.6 mmol) in methanol was added thionyl chloride (0.95 mL, 12.7 mmol) and the reaction was stirred at room temperature overnight. Concentration followed by trituration with ether gives a white solid. The solid is filtered, washed with ether and dried to afford the desired product (3.5 g, 10 mmol, 95%) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ 8.79 (br, 2H), 8.01 (s, 1H), 7.74 (d, J=8.1 Hz, 1H). 7.57 (d, J=7.8 Hz, 1H), 7.21 (dd, J=8.1, 7.8 Hz, 1H), 4.56 (br, 1H), 3.54 (s, 3H), 3.23-3.17 (m, 1H), 3.04-2.98 (m, 1H).

후처리

  1. concentrationConcentration
  2. customgives a white solid
  3. filtrationThe solid is filtered
  4. washwashed with ether
  5. customdried

출처 및 근거

ORD 기록
ord-ac3dc423ba244e298f2c0f526680be5a
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08058449B2

반응 노트

불러오는 중…