Borane → (1-Tert-butyl-piperidin-4-yl)-hydrazine

HRID 2109272ノート

反応式

HRID 2109272 の反応式
B.C1COCC1.C(OC([NH:14][N:15]=[C:16]1[CH2:21][CH2:20][N:19]([C:22]([CH3:25])([CH3:24])[CH3:23])[CH2:18][CH2:17]1)=O)(C)(C)C>Cl>[C:22]([N:19]1[CH2:18][CH2:17][CH:16]([NH:15][NH2:14])[CH2:21][CH2:20]1)([CH3:25])([CH3:23])[CH3:24]

参加物

5

反応物 3

HCID 6331BoraneHCID 8028TetrahydrofuranHCID 48916874Tert-butyl 2-(1-tert-butylpiperidin-4-ylidene)hydrazinecarboxylate

生成物 1

HCID 21097250(1-Tert-butyl-piperidin-4-yl)-hydrazine

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
60 °C

実験手順

A 1M solution borane in THF (28.7 mL, 28.7 mmol) was added to N′-(1-tert-Butyl-piperidin-4-ylidene)-hydrazinecarboxylic acid tert-butyl ester. The mixture was stirred for 16 h, and then 40 mL of 6M HCl was added. The mixture was heated to 60° C. for 30 min. The mixture was concentrated and 200 mL of petroleum ether was added, followed by powdered NaOH (5 g). The slurry was stirred manually for 30 min, and then the mixture was dried with MgSO4, filtered, and concentrated to give 1.21 g of (1-tert-butyl-piperidin-4-yl)-hydrazine (1.21 g).

後処理

  1. concentrationThe mixture was concentrated
  2. addition200 mL of petroleum ether was added
  3. stirringThe slurry was stirred manually for 30 min
  4. dry with materialthe mixture was dried with MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-b9e6f9eca0e3440ab86fb9bf9bcafa43
出典データセット
uspto-grants-2009_04
特許番号
US07514458B2

反応ノート

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