Hydrochloric Acid → N-(6-benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-yl)-N'-methyl-ethane-1,2-diamine

HRID 2103348ノート

反応式

HRID 2103348 の反応式
C(O[C:6](=O)[N:7]([CH2:9][CH2:10][NH:11][CH:12]1[C:21]2[C:16](=[CH:17][C:18]([S:22]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)(=[O:24])=[O:23])=[CH:19][CH:20]=2)[CH2:15][CH2:14][CH2:13]1)C)(C)(C)C.Cl>O1CCCC1.CCOCC>[C:25]1([S:22]([C:18]2[CH:17]=[C:16]3[C:21](=[CH:20][CH:19]=2)[CH:12]([NH:11][CH2:10][CH2:9][NH:7][CH3:6])[CH2:13][CH2:14][CH2:15]3)(=[O:23])=[O:24])[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 57804253[2-(6-Benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-ylamino)-ethyl]-methyl-carbamic acid tert-butyl ester

生成物 1

HCID 11523041N-(6-benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-yl)-N'-methyl-ethane-1,2-diamine収率 97%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

[2-(6-Benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-ylamino)-ethyl]-methyl-carbamic acid tert-butyl ester (0.4 g, 0.9 mmol) was dissolved in 20 mL of tetrahydrofuran, and 20 mL of 10% HCl in Et2O was added. The reaction mixture was refluxed for one hour and then cooled. The solvent was evaporated under reduced pressure, and the resulting solid was recrystallized from EtOH-Et2O to yield 0.3 g (0.87 mmol, 97%) of N-(6-benzenesulfonyl-1,2,3,4-tetrahydro-naphthalen-1-yl)-N′-methyl-ethane-1,2-diamine as a hydrochloride salt. MS: 345 (M+H)+.

後処理

  1. temperatureThe reaction mixture was refluxed for one hour
  2. temperaturecooled
  3. customThe solvent was evaporated under reduced pressure
  4. customthe resulting solid was recrystallized from EtOH-Et2O

出典と根拠

ORDレコード
ord-63fca4eb8c8a49d49282f6213f684e74
出典データセット
uspto-grants-2009_08
特許番号
US07576103B2

反応ノート

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