Ammonia → HCID 57931184、化合物

HRID 551160ノート

反応式

HRID 551160 の反応式
[CH2:1]([S:3]([N:6]1[CH2:11][CH2:10][C:9]([CH2:14][CH:15]2[CH2:19][CH2:18][CH2:17][O:16]2)([C:12]#[N:13])[CH2:8][CH2:7]1)(=[O:5])=[O:4])[CH3:2].N.O>CO.[Ni]>[CH2:1]([S:3]([N:6]1[CH2:11][CH2:10][C:9]([CH2:12][NH2:13])([CH2:14][CH:15]2[CH2:19][CH2:18][CH2:17][O:16]2)[CH2:8][CH2:7]1)(=[O:5])=[O:4])[CH3:2]

参加物

6

反応物 3

HCID 222AmmoniaHCID 962WaterHCID 579311911-(Ethylsulfonyl)-4-[(tetrahydro-2-furanyl)methyl]-4-piperidinecarbonitrile

生成物 1

HCID 57931184HCID 57931184、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

In a heavy wall flask was placed 1-(ethylsulfonyl)-4-(tetrahydrofuran-2-ylmethyl)piperidine-4-carbonitrile (15, 2 g, 6.98 mmol) and 2N ammonia in methanol (50 ml). To this was added commercially available Raney nickel slurry in water (1.8 g, 20.94 mmol) and the solution agitated under hydrogen atmosphere (45 psi) at room temp for 12 hours. The catalyst was filtered off using celite and washed with MeOH (200 ml) and the combined organics concentrated in vacuo to give 1-[1-(ethylsulfonyl)-4-(tetrahydrofuran-2-ylmethyl)piperidin-4-yl]methanamine (16) as a clear semi-solid. MS 291 (M+1)

後処理

  1. customIn a heavy wall flask was placed
  2. filtrationThe catalyst was filtered off
  3. washwashed with MeOH (200 ml)
  4. concentrationthe combined organics concentrated in vacuo

出典と根拠

ORDレコード
ord-d16466a8126c408896b4f3761a16d860
出典データセット
uspto-grants-2011_05
特許番号
US07947714B2

反応ノート

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