Hydrazine hydrate (1:1) → 4-[4-(2-tert-Butyl-6-cyclobutyl-pyrimidin-4-yl)piperazin-1-yl]-butylamine

HRID 219699노트

반응식

HRID 219699 반응식
[C:1]([C:5]1[N:10]=[C:9]([N:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][CH2:19][CH2:20][N:21]3C(=O)C4C(=CC=CC=4)C3=O)[CH2:13][CH2:12]2)[CH:8]=[C:7]([CH:32]2[CH2:35][CH2:34][CH2:33]2)[N:6]=1)([CH3:4])([CH3:3])[CH3:2].O.NN>C(O)C>[C:1]([C:5]1[N:10]=[C:9]([N:11]2[CH2:12][CH2:13][N:14]([CH2:17][CH2:18][CH2:19][CH2:20][NH2:21])[CH2:15][CH2:16]2)[CH:8]=[C:7]([CH:32]2[CH2:35][CH2:34][CH2:33]2)[N:6]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 690260812-{4-[4-(2-tert-Butyl-6-cyclobutyl-pyrimidin-4-yl)-piperazin-1-yl]-butyl}-isoindole-1,3-dione

생성물 1

HCID 690260674-[4-(2-tert-Butyl-6-cyclobutyl-pyrimidin-4-yl)piperazin-1-yl]-butylamine수율 68.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2.4 g of 2-{4-[4-(2-tert-butyl-6-cyclobutyl-pyrimidin-4-yl)-piperazin-1-yl]-butyl}-isoindole-1,3-dione (5.05 mmol) and 1.0 g of hydrazine hydrate (20.2 mmol) were dissolved in 20 ml of ethanol and heated to reflux for 1 h. The precipitate was filtered and the filtrate extracted with water and ethyl acetate. The organic layer was dried over magnesium sulfate, filtered, and concentrated to dryness to yield 1.2 g of the title compound.

후처리

  1. temperatureheated
  2. temperatureto reflux for 1 h
  3. filtrationThe precipitate was filtered
  4. extractionthe filtrate extracted with water and ethyl acetate
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-53e301ff681744bb85772887fb338a00
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08202868B2

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