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Hydrochloric Acid → N2-(2,6-Dimethyl-4-pyridyl)propane-1,2-diamine hydrochloride

HRID 333082
ノート
印刷プレビュー

反応式

HRID 333082 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([NH:8][CH:9]([CH3:19])[CH2:10][NH:11]C(=O)OC(C)(C)C)[CH:5]=[C:4]([CH3:20])[N:3]=1.[ClH:21]>O1CCOCC1>[ClH:21].[CH3:1][C:2]1[CH:7]=[C:6]([NH:8][CH:9]([CH3:19])[CH2:10][NH2:11])[CH:5]=[C:4]([CH3:20])[N:3]=1
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 2

HCID 313Hydrochloric AcidHCID 86691169Tert-butyl 2-(2,6-dimethylpyridin-4-ylamino)propylcarbamate

生成物 1

HCID 66835507N2-(2,6-Dimethyl-4-pyridyl)propane-1,2-diamine hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To tert-butyl 2-(2,6-dimethylpyridin-4-ylamino)propylcarbamate (147 mg, 0.526 mmol) dissolved in 1,4-dioxane (1 ml) a 4N solution of HCl in dioxane (2 ml, 8.00 mmol) was added. Within a few minutes a precipitate started to form. The solvent was removed in a stream of nitrogen, to the residue was added diethylether and the mixture was allowed to stand at room temperature overnight. The solvent was filtered off, the residue was dried under reduced pressure to yield 135 mg of an off-white solid MS (ESI) m/z=180.0.

後処理

  1. additionwas added
  2. waitWithin a few minutes a precipitate started
  3. customto form
  4. customThe solvent was removed in a stream of nitrogen, to the residue
  5. additionwas added diethylether
  6. filtrationThe solvent was filtered off
  7. customthe residue was dried under reduced pressure

出典と根拠

ORDレコード
ord-23b3de78bbb24b248281e8b8438fb5c3
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877934B2

反応ノート

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