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HCID 178424364、化合物 → 2-methyl-N-[(1R)-1-phenylethyl]cyclohexan-1-amine

HRID 62659
ノート
印刷プレビュー

反応式

HRID 62659 の反応式
[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][CH2:4]/[C:3]/1=[N:8]\[C@@H:9]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[CH3:10]>C(O)C.[Ni]>[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[NH:8][C@@H:9]([C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)[CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 178424364HCID 178424364、化合物

生成物 1

HCID 127142172-methyl-N-[(1R)-1-phenylethyl]cyclohexan-1-amine収率 80%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

A suspension of (1R,E)-N-(2-methylcyclohexylidene)-1-phenylethanamine (I-8a: 25 g, 116.27 mmol) and Raney-Ni (3.75 g) in ethanol (250 mL) was maintained under hydrogen atmosphere in a Parr hydrogenator using 5 bar pressure for 2 days. The reaction mixture was filtered and filtrate evaporated under reduced pressure. The crude compound was treated with ethereal HCl, and the precipitated salt was filtered, washed with cold ether and dried to afford 20 g (80%) of 2-methyl-N—((R)-1-phenylethyl)-cyclohexanamine (I-8b) as a white solid.

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. temperaturewas maintained under hydrogen atmosphere in a Parr hydrogenator
  2. customfor 2 days
  3. filtrationThe reaction mixture was filtered
  4. customfiltrate evaporated under reduced pressure
  5. additionThe crude compound was treated with ethereal HCl
  6. filtrationthe precipitated salt was filtered
  7. washwashed with cold ether
  8. customdried

出典と根拠

ORDレコード
ord-350460199f344be4b1b3c00607a63c82
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09447039B2

反応ノート

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