Methylamine → 2-(2-aminoethyl)-8H-indeno[1,2-d]thiazole fumarate

HRID 356114

反応式

HRID 356114 の反応式
C1(=O)[N:5]([CH2:6][CH2:7][C:8]2[S:9][C:10]3[CH2:19][C:18]4[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=4[C:11]=3[N:12]=2)C(=O)C2=CC=CC=C12.CN.[C:28]([OH:35])(=[O:34])/[CH:29]=[CH:30]/[C:31]([OH:33])=[O:32]>CO>[C:28]([OH:35])(=[O:34])/[CH:29]=[CH:30]/[C:31]([OH:33])=[O:32].[NH2:5][CH2:6][CH2:7][C:8]1[S:9][C:10]2[CH2:19][C:18]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[C:11]=2[N:12]=1

参加物

5

反応物 3

HCID 6329MethylamineHCID 444972Fumaric AcidHCID 189409522-(2-Phthalimidoethyl)-8H-indeno[1,2-d]thiazole

生成物 1

HCID 189410722-(2-aminoethyl)-8H-indeno[1,2-d]thiazole fumarate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

実験手順

In 20 ml of methanol, 1.79 g of 2-(2-phthalimidoethyl)-8H-indeno[1,2-d]thiazole was dissolved. Then, 40 ml of a 40% solution of methylamine in methanol was added, followed by stirring at room temperature for 14 hours. The solvent was then evaporated, and chloroform and 1N hydrochloric acid were added to the resulting residue. The aqueous layer was separated and then neutralized with a 1N aqueous solution of sodium hydroxide, followed by extraction with chloroform. The chloroform layer separated was washed successively with water and a saturated aqueous solution of sodium chloride, followed by drying over anhydrous sodium sulfate. The residue obtained by evaporation of the solvent was dissolved in methanol, and fumaric acid was added thereto. The crystals formed were collected by filtration and then washed successively with methanol and diethyl ether, followed by recrystallization from methanol, whereby 572 mg of 2-(2-aminoethyl)-8H-indeno[1,2-d]thiazole fumarate was obtained.

後処理

  1. customThe solvent was then evaporated
  2. additionchloroform and 1N hydrochloric acid were added to the resulting residue
  3. customThe aqueous layer was separated
  4. extractionfollowed by extraction with chloroform
  5. customThe chloroform layer separated
  6. washwas washed successively with water
  7. dry with materialby drying over anhydrous sodium sulfate
  8. customThe residue obtained by evaporation of the solvent
  9. customThe crystals formed
  10. filtrationwere collected by filtration
  11. washwashed successively with methanol and diethyl ether
  12. customfollowed by recrystallization from methanol

出典と根拠

ORDレコード
ord-7945e8998fb046cf81c5b7e2c8fa4361
出典データセット
uspto-grants-1998_11
特許番号
US05834499

関連ノート

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