Hydrazine → 4-[6-(3-Amino-propyl)-pyridin-3-yl]-butyl amine

HRID 993244

反応式

HRID 993244 の反応式
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[CH2:12][CH2:13][CH2:14][CH2:15][C:16]1[CH:17]=[CH:18][C:19]([CH2:22][CH2:23][CH2:24][N:25]2C(=O)C3C(=CC=CC=3)C2=O)=[N:20][CH:21]=1.NN>C(O)C>[NH2:25][CH2:24][CH2:23][CH2:22][C:19]1[N:20]=[CH:21][C:16]([CH2:15][CH2:14][CH2:13][CH2:12][NH2:3])=[CH:17][CH:18]=1

参加物

4

反応物 2

HCID 9321HydrazineHCID 184089852-(3-{5-[4-(1,3-Dioxo-isoindol-2-yl)-butyl]-pyridin-2-yl}-propyl)-isoindole-1,3-dione

生成物 1

HCID 184089864-[6-(3-Amino-propyl)-pyridin-3-yl]-butyl amine収率 111.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 3-4 (14 g, 30.7 mmol) and hydrazine (5 mL) in ethanol (500 mL) was heated at reflux for 5 hours. The mixture was cooled and concentrated to ⅓ volume, diluted with 300 mL MTBE, and filtered. The filtrate was concentrated to give 7.1 g of 3-5 as a brown oil, contaminated with a small amount of phthalhydrazide.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 5 hours
  3. temperatureThe mixture was cooled
  4. concentrationconcentrated
  5. additiondiluted with 300 mL MTBE
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-165f3f74c3344296a55b0036b226de24
出典データセット
uspto-grants-2002_10
特許番号
US06472403B2

関連ノート

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