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HRID1088924

反应详情

EQUATION

反应方程式

HRID 1088924 反应方程式

REACTANTS

反应物

3
Hydrochloric Acid 分子结构式
HCID313

Hydrochloric Acid

ClH

Water 分子结构式
HCID962

Water

H2O

N-(2,2-Diethoxyethyl)-N-[(4-methoxy-1,3-benzodioxol-5-yl)methyl]-4-methylbenzenesulfonamide 分子结构式
HCID13911325

N-(2,2-Diethoxyethyl)-N-[(4-methoxy-1,3-benzodioxol-5-yl)methyl]-4-methylbenzenesulfonamide

C22H29NO7S

PRODUCTS

产物

1
4-Methoxy-2H-[1,3]dioxolo[4,5-g]isoquinoline--hydrogen chloride (1/1) 分子结构式
HCID70364587

4-Methoxy-2H-[1,3]dioxolo[4,5-g]isoquinoline--hydrogen chloride (1/1)

C11H10ClNO3

收率 61.8%

AUXILIARIES

试剂、催化剂与溶剂

1
1,4-Dioxane 分子结构式
溶剂HCID31275

1,4-Dioxane

C4H8O2

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

N-(2-methoxy-3,4-methylenedioxybenzyl)-N-(p-toluenesulfonyl)aminoacetaldehyde diethylacetal (3) in an amount of 69.89 g (0.155 mol) was dissolved in 0.194 ml of dioxane, to which 14.7 ml (0.169 mol) of concentrated hydrochloric acid and 47.1 ml of water were added and heated under reflux for two hours and 40 minutes. After the mixture were cooled to about 5° C., deposited crystals were collected by filtration, washed with 30 ml of cold dioxcane and then dried to obtain 22.95 g of 8-methoxy-6,7-methylenedioxyisoquinoline hydrochloride (4) as yellow crystals. Yield 61.8%.

WORKUP

后处理

  1. additionwere added
  2. temperatureheated
  3. temperatureunder reflux for two hours and 40 minutes
  4. filtrationwere collected by filtration
  5. washwashed with 30 ml of cold dioxcane
  6. customdried