Pyrrolidine → HCID 178456693, 화합물

반응식

C([O:3][C:4]([NH:6][N:7]([CH:10]([CH3:12])[CH3:11])[C:8]#[N:9])=O)C.[NH:13]1[CH2:17][CH2:16][CH2:15][CH2:14]1>>[CH:10]([N:7]1[C:8]([N:13]2[CH2:17][CH2:16][CH2:15][CH2:14]2)=[N:9][C:4]([OH:3])=[N:6]1)([CH3:12])[CH3:11]

참가 물질

반응물 2

HCID 31268Pyrrolidine

HCID 19390523HCID 19390523, 화합물

생성물 1

HCID 178456693HCID 178456693, 화합물수율 70%

반응 조건

온도: 30 °C

실험 절차

26,6 g (0,15 mole) of 2-isopropyl-2-cyanohydrazinecarboxylic acid ethyl ester is added dropwise to 100 ml of pyrrolidine. The temperature raises to 30° C during the dropwise addition. The whole mixture is then stirred for 12 hours at room temperature and subsequently for 1 hour at 70° C. Then excess pyrrolidine is distilled off in vacuo. To the crystalline residue ethyl acetate is added and the crystals are filtered with suction. There is obtained 21,6 g (70% of theory) of 1-isopropyl-3-hydroxy-5-pyrrolidino-1,2,4-triazole, mp. 123°-125° C.

후처리

distillationThen excess pyrrolidine is distilled off in vacuo
additionTo the crystalline residue ethyl acetate is added
filtrationthe crystals are filtered with suction

출처 및 근거

ORD 기록: ord-44062f9a01ad43dc9835a5d723b3fded
출처 데이터셋: uspto-grants-1978_02
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04076938

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