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Acetyl chloride → N-Methyl-1-(1-(pyrimidin-4-yl)piperidin-4-yl)methanamine dihydrochloride

HRID 1193345
ノート
印刷プレビュー

反応式

HRID 1193345 の反応式
[CH3:1][N:2]([CH2:10][CH:11]1[CH2:16][CH2:15][N:14]([C:17]2[CH:22]=[CH:21][N:20]=[CH:19][N:18]=2)[CH2:13][CH2:12]1)C(=O)OC(C)(C)C.C([Cl:26])(=O)C>C(O)C>[ClH:26].[ClH:26].[CH3:1][NH:2][CH2:10][CH:11]1[CH2:12][CH2:13][N:14]([C:17]2[CH:22]=[CH:21][N:20]=[CH:19][N:18]=2)[CH2:15][CH2:16]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6367Acetyl chlorideHCID 66805336tert-Butyl methyl((1-(pyrimidin-4-yl)piperidin-4-yl)methyl)carbamate

生成物 1

HCID 66798692N-Methyl-1-(1-(pyrimidin-4-yl)piperidin-4-yl)methanamine dihydrochloride収率 99%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
40 °C

実験手順

tert-Butyl methyl((1-(pyrimidin-4-yl)piperidin-4-yl)methyl)carbamate (0.718 mmol, 1 eq) was dissolved in ethanol (2.5 ml), and acetyl chloride (3.59 mmol, 5.0 eq) was added while cooling with ice. The reaction mixture was then stirred for 2 hours at 40° C. and then concentrated. The residue was taken up in a small amount of acetone and a solid was precipitated with diethyl ether. The solid was filtered off, washed with diethyl ether and dried. Yield: >99%

後処理

  1. temperaturewhile cooling with ice
  2. concentrationconcentrated
  3. customa solid was precipitated with diethyl ether
  4. filtrationThe solid was filtered off
  5. washwashed with diethyl ether
  6. customdried

出典と根拠

ORDレコード
ord-1d5fad775833418faffb680582c90113
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08680159B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート