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

HRID 27771

反応式

HRID 27771 の反応式
[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

参加物

5

反応物 3

HCID 313Hydrochloric Acid3 回HCID 695242,2-DiethoxyethylamineHCID 819113,4-Dimethoxyphenethyl alcohol

生成物 1

HCID 122258846,7-Dimethoxy-1-isochromanmethylamine

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-1e2f3cdde0d746b2b8d98ffbdef4111e
出典データセット
uspto-grants-1980_09
特許番号
US04223151

関連ノート

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