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Ammonia → 2-Isopropoxy-2-(2-methylpyrimidin-5-yl)ethanamine

HRID 512201
ノート
印刷プレビュー

反応式

HRID 512201 の反応式
[CH:1]([O:4][CH:5]([C:8]1[CH:9]=[N:10][C:11]([CH3:14])=[N:12][CH:13]=1)[C:6]#[N:7])([CH3:3])[CH3:2].N>CO.[Ni]>[CH:1]([O:4][CH:5]([C:8]1[CH:9]=[N:10][C:11]([CH3:14])=[N:12][CH:13]=1)[CH2:6][NH2:7])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 222AmmoniaHCID 867162292-Isopropoxy-2-(2-methylpyrimidin-5-yl)acetonitrile

生成物 1

HCID 867162282-Isopropoxy-2-(2-methylpyrimidin-5-yl)ethanamine

試薬・触媒・溶媒 2

HCID 935Nickel触媒2 回HCID 887Methanol溶媒2 回

実験手順

2-Isopropoxy-2-(2-methylpyrimidin-5-yl)acetonitrile (169 mg, 0.884 mmol) was dissolved in methanol (10 ml) and 7M NH3 in methanol (4 ml). Argon was bubbled through the solution for 5 minutes. To the reaction was added Raney nickel (100 mg, 1.704 mmol) and it was fitted with a H2-filled balloon. After stirring at room temperature for 20 hours LCMS shows only around 30% conversion and raney nickel (100 mg, 1.70 mmol) was added. The reaction was stirred for another 72 hours, then filtered through a plug of celite and concentrated in vacuo. The crude product used for next reaction without further purification.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customArgon was bubbled through the solution for 5 minutes
  2. customwas fitted with a H2-
  3. additionfilled balloon
  4. additionwas added
  5. stirringThe reaction was stirred for another 72 hours
  6. filtrationfiltered through a plug of celite and
  7. concentrationconcentrated in vacuo
  8. customThe crude product used for next reaction without further purification

出典と根拠

ORDレコード
ord-7c83b31eef824ee892e25ac7a42251da
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09102591B2

反応ノート

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