Hydrochloric Acid → 6,7-Dimethoxy-1-isochromanmethylamine

HRID 27771

반응식

HRID 27771 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[O:12][CH3:13])[CH2:6][CH2:7][OH:8].C(O[CH:17](OCC)[CH2:18][NH2:19])C.Cl>O1CCOCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[CH:17]([CH2:18][NH2:19])[O:8][CH2:7][CH2:6]2

참가 물질

5

반응물 3

HCID 313Hydrochloric Acid3회HCID 695242,2-DiethoxyethylamineHCID 819113,4-Dimethoxyphenethyl alcohol

생성물 1

HCID 122258846,7-Dimethoxy-1-isochromanmethylamine

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of the starting material of formula II, 3,4-dimethoxyphenethyl alcohol (108 g), described by E. Z. Khafagy and J. P. Lambooy, J. Med. Chem. 9, 936 (1966), and the starting material of formula III, aminoacetaldehyde diethyl acetal (78 g), in dry dioxane (250 ml) is stirred and cooled (ice bath) while being saturated with hydrogen chloride over a period of one hour. The mixture is kept at room temperature for two days. The crystalline precipitate is collected, washed with dry dioxane and then ether to yield the hydrochloric acid addition salt (hydrochloride) of the title compound, m.p. 250°-255° C. (dec.), after recrystallization from methanol.

후처리

  1. temperaturecooled (ice bath)
  2. customThe crystalline precipitate is collected
  3. washwashed with dry dioxane
  4. customether to yield

출처 및 근거

ORD 기록
ord-1e2f3cdde0d746b2b8d98ffbdef4111e
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04223151

연결된 노트

불러오는 중…