Hydrochloric Acid → (R)-4-(3,4-dichlorophenyl)butan-2-amine hydrochloride

HRID 1844422ノート

反応式

HRID 1844422 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][C@H:11]([NH:13][S@](C(C)(C)C)=O)[CH3:12])[CH:5]=[CH:6][C:7]=1[Cl:8].Cl.CC(S(OC)=O)(C)C>CO.O1CCOCC1>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][C@H:11]([NH2:13])[CH3:12])[CH:5]=[CH:6][C:7]=1[Cl:8]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 543690Methyl 2-methylpropane-2-sulfinateHCID 86731088(S)-N-((R)-4-(3,4-dichlorophenyl)butan-2-yl)-2-methylpropane-2-sulfinamide

生成物 1

HCID 86731090(R)-4-(3,4-dichlorophenyl)butan-2-amine hydrochloride収率 195%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

(S)-N-((R)-4-(3,4-Dichlorophenyl)butan-2-yl)-2-methylpropane-2-sulfinamide (600 mg, 1.862 mmol) was stirred in MeOH (10 mL) at rt. 4N HCl in dioxane (5 mL) was added. The resulting mixture was stirred at rt for 20 min. The solvents were evaporated and CH2Cl2 (3×) was added and evaporated. The resulting white solids were vacuum dried for 5 h to give (R)-4-(3,4-dichlorophenyl)butan-2-amine hydrochloride (462 mg, 1.815 mmol, 97% yield) as off-white solids and methyl 2-methylpropane-2-sulfinate. The HCl salt was used without further purification. LC-MS (ESI) m/z 218.0 (M+H), RT=1.61 min (Method B).

後処理

  1. customThe solvents were evaporated
  2. additionCH2Cl2 (3×) was added
  3. customevaporated
  4. customdried for 5 h

出典と根拠

ORDレコード
ord-5dde90ca36fa4799bb65d4894654b4b7
出典データセット
uspto-grants-2015_02
特許番号
US08946430B2

反応ノート

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