Water → N-(2,2-Dimethoxyethyl)-4-methoxy-N-methyl-1,3-benzodioxole-5-methanamine

HRID 622198ノート

反応式

HRID 622198 の反応式
[CH2:1]([O:3][CH:4]([O:29][CH2:30]C)[CH2:5][N:6]([CH2:17][C:18]1[CH:23]=[CH:22][C:21]2[O:24][CH2:25][O:26][C:20]=2[C:19]=1[O:27][CH3:28])S(C1C=CC(C)=CC=1)(=O)=O)C.O.[OH-].[Na+].[CH2:35](Cl)Cl>>[CH3:30][O:29][CH:4]([O:3][CH3:1])[CH2:5][N:6]([CH2:17][C:18]1[CH:23]=[CH:22][C:21]2[O:24][CH2:25][O:26][C:20]=2[C:19]=1[O:27][CH3:28])[CH3:35]

参加物

5

反応物 4

HCID 962WaterHCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 13911325N-(2-methoxy-3,4-methylenedioxybenzyl)-N-(p-toluenesulfonyl)aminoacetaldehyde diethylacetal

生成物 1

HCID 14609557N-(2,2-Dimethoxyethyl)-4-methoxy-N-methyl-1,3-benzodioxole-5-methanamine収率 99.7%

実験手順

17.8 g (74.3 mmol) of the compound (2) thus obtained was added to 50 ml of water, to which 100 ml of methylene chloride was added. This solution was made basic with 25% aqueous solution of sodium hydroxide under water-cooling. The solution was separated and the aqueous layer was extracted with 20 ml of methylene chloride. The obtained methylene chloride layers were combined, washed with 30 ml of water, dried over anhydrous magnesium sulfate and then concentrated under vacuum to obtain 15.06 g of 8-methoxy-6,7-methylenedioxyisoquinoline (3) (yield 99.7%). The product thus obtained was recrystallized from ethylacetate-n-hexane, m.p. 144°-5° C. IR and NMR spectra of the resultant product are listed below. ##STR48##

後処理

  1. additionwas added
  2. temperaturecooling
  3. customThe solution was separated
  4. extractionthe aqueous layer was extracted with 20 ml of methylene chloride
  5. washwashed with 30 ml of water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-be23a90f2ef54c33add335383e7cbb18
出典データセット
uspto-grants-1988_09
特許番号
US04769480

反応ノート

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