Chloride → 3-(4-Aminobenzyl)-thiazolidine

HRID 1244493ノート

反応式

HRID 1244493 の反応式
[N+:1]([C:4]1[CH:15]=[CH:14][C:7]([CH2:8][N:9]2[CH2:13][CH2:12][S:11][CH2:10]2)=[CH:6][CH:5]=1)([O-])=O.[Cl-]>Cl>[NH2:1][C:4]1[CH:15]=[CH:14][C:7]([CH2:8][N:9]2[CH2:13][CH2:12][S:11][CH2:10]2)=[CH:6][CH:5]=1

参加物

4

反応物 2

HCID 312ChlorideHCID 219186763-(4-Nitrobenzyl)-thiazolidine

生成物 1

HCID 154105273-(4-Aminobenzyl)-thiazolidine収率 63%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

3-(4-nitrobenzyl)-thiazolidine (1.1 g, 5 mmoles) is put into solution in 10 ml concentrated hydrochloric acid at 0° C. Dihydrated in chloride (7.7g, 34 mmoles) is added in portions, the mixture is heated for 2 hours under reflux and the acid is evaporated off under reduced pressure. The residue is then taken up in 20 ml of water and. neutralized with a 2N soda solution (approximately 100 ml). 100 ml of dichloromethane is added to the medium and the whole is filtered on celite in order to eliminate the salts in suspension. The organic phase is extracted, washed 3 times with 50 ml of water, dried, filtered and evaporated to dryness under reduced pressure. The expected product is purified on silica gel in a dichloromethane/methanol (98/2) mixture and is obtained in the form of of a beige powder (0.6 g, 63%). Melting point: 73-74° C.

後処理

  1. additionis added in portions
  2. temperaturethe mixture is heated for 2 hours
  3. temperatureunder reflux
  4. customthe acid is evaporated off under reduced pressure
  5. addition100 ml of dichloromethane is added to the medium
  6. filtrationthe whole is filtered on celite in order
  7. extractionThe organic phase is extracted
  8. washwashed 3 times with 50 ml of water
  9. customdried
  10. filtrationfiltered
  11. customevaporated to dryness under reduced pressure
  12. customThe expected product is purified on silica gel in a dichloromethane/methanol (98/2) mixture

出典と根拠

ORDレコード
ord-4002823f987545829f28dd53878ef30b
出典データセット
uspto-grants-2006_10
特許番号
US07122535B2

反応ノート

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