Carbamimidoylazanium Chloride → HCID 178462846, 화합물

HRID 1792906

반응식

HRID 1792906 반응식
CC(C)([O-])C.[K+].[Cl-].[NH2:8][C:9]([NH2:11])=[NH2+:10].[CH2:12]([N:14]1[C:22](=[O:23])[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]1[CH2:24][C:25](OCC)=[O:26])[CH3:13]>O>[CH2:12]([N:14]1[C:22](=[O:23])[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]1[CH2:24][C:25]([NH:10][C:9]([NH2:11])=[NH:8])=[O:26])[CH3:13]

참가 물질

5

반응물 3

HCID 5460839Carbamimidoylazanium ChlorideHCID 23665647Potassium tert-butoxideHCID 86591360ethyl (2-ethyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate

생성물 1

HCID 178462846HCID 178462846, 화합물수율 28%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
20 °C

실험 절차

N-[(2-Ethyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetyl]guanidine is prepared as described in Example 1, starting with 4.3 g of potassium tert-butoxide, 3.7 g of guanidinium chloride and 1.9 g of ethyl (2-ethyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate. The reaction mixture is stirred at a temperature in the region of 20° C. for 20 hours, followed by addition of 60 cm3 of water. The aqueous phase is extracted with 3 times 50 cm3 of ethyl acetate and is then concentrated to dryness under reduced pressure (0.6 kPa) at a temperature in the region of 45° C. The residue is taken up in water, triturated and filtered. The solid is taken up in methanol and the solvent is then evaporated to dryness under reduced pressure (0.6 kPa) at a temperature in the region of 45° C. 0.56 g of N-[(2-ethyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetyl]-guanidine is thus obtained in the form of an off-white solid melting at 223° C. Mass spectrum EI: m/e 260 (M+), m/e 173, m/e 160, m/e 132.

후처리

  1. customN-[(2-Ethyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetyl]guanidine is prepared
  2. extractionThe aqueous phase is extracted with 3 times 50 cm3 of ethyl acetate
  3. concentrationis then concentrated to dryness under reduced pressure (0.6 kPa) at a temperature in the region of 45° C
  4. customtriturated
  5. filtrationfiltered
  6. customthe solvent is then evaporated to dryness under reduced pressure (0.6 kPa) at a temperature in the region of 45° C

출처 및 근거

ORD 기록
ord-3070f13bd72545d38a8514b0b4057615
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07078428B2

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