Methanesulfonic Acid → Methanesulfonic acid--(3R)-3-aminopentanenitrile (1/1)

HRID 2120330ノート

反応式

HRID 2120330 の反応式
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].C(OC(=O)[NH:12][CH:13]([CH2:16][C:17]#[N:18])[CH2:14][CH3:15])(C)(C)C>O1CCCC1>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[NH2:12][C@H:13]([CH2:14][CH3:15])[CH2:16][C:17]#[N:18]

参加物

4

反応物 2

HCID 6395Methanesulfonic AcidHCID 21629520tert-butyl N-(1-cyanobutan-2-yl)carbamate

生成物 1

HCID 57350099Methanesulfonic acid--(3R)-3-aminopentanenitrile (1/1)

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

Methane sulfonic acid (71 g) was added to a solution of (1-cyanomethyl-propyl)-carbamic acid tert-butyl ester in tetrahydrofuran (530 mL). The reaction mixture was heated to 40° C. for approximately 30 minutes. The temperature was raised to 45° C. and stirred for approximately one hour. The temperature was raised again to 65° C. and the reaction mixture was stirred for five hours. The mixture was allowed to cool to ambient temperature. The resulting solids were isolated by filtration to afford the title compound (41.53 g).

後処理

  1. temperatureThe temperature was raised to 45° C.
  2. temperatureThe temperature was raised again to 65° C.
  3. stirringthe reaction mixture was stirred for five hours
  4. temperatureto cool to ambient temperature
  5. customThe resulting solids were isolated by filtration

出典と根拠

ORDレコード
ord-4050e2d968e6450ca602020bbad682f6
出典データセット
uspto-grants-2004_02
特許番号
US06689897B2

反応ノート

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