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

HRID 512201
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HRID 512201 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 935Nickel촉매2회HCID 887Methanol용매2회

실험 절차

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.

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후처리

  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

출처 및 근거

ORD 기록
ord-7c83b31eef824ee892e25ac7a42251da
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09102591B2

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