Hydrochloric Acid → HCID 178449906, 화합물

HRID 1794584

반응식

HRID 1794584 반응식
[ClH:1].[C:2](=[NH:9])(OCC)[CH2:3][CH2:4][CH3:5].C(N(CC)CC)C.[CH2:17]([O:19][C:20]1[CH:29]=[CH:28][CH:27]=[CH:26][C:21]=1[C:22]([NH:24][NH2:25])=[O:23])[CH3:18].C(=N)(OCC)CCC.Cl>C(O)(C)C>[ClH:1].[NH:9]=[C:2]([NH:25][NH:24][C:22](=[O:23])[C:21]1[CH:26]=[CH:27][CH:28]=[CH:29][C:20]=1[O:19][CH2:17][CH3:18])[CH2:3][CH2:4][CH3:5]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 16634Ethyl butyrimidateHCID 1407882-EthoxybenzhydrazideHCID 12235055Ethyl butyrimidate hydrochloride

생성물 1

HCID 178449906HCID 178449906, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
0 °C

실험 절차

Ethyl butyrimidate hydrochloride from Example B (71.5 g, 472 mmol) is introduced into triethylamine (65 ml, 472 mmol) and cooled to 0° C. 2-Ethoxybenzohydrazide from Example A (85 g, 472 mmol) is suspended in 250 ml of isopropanol and added to the ethyl butyrimidate mixture. The reaction mixture is stirred at room temperature for 48 hours, the solid (triethylamine hydrochloride) is removed, and 25% strength hydrochloric acid (150 ml, 1.18 mol) is slowly added dropwise to the mother liquor at 0° C. to 5° C. The suspension of crystals is then stirred at 0° C. to 5° C. for 1 hour and the crystals are filtered with suction through a sintered funnel, washed with 100 ml of cold isopropanol and dried in a vacuum oven at 30° C. and 300 mbar overnight.

후처리

  1. customthe solid (triethylamine hydrochloride) is removed
  2. additionThe suspension of crystals
  3. stirringis then stirred at 0° C. to 5° C. for 1 hour
  4. filtrationthe crystals are filtered with suction through a sintered funnel
  5. washwashed with 100 ml of cold isopropanol
  6. customdried in a vacuum oven at 30° C.
  7. custom300 mbar overnight

출처 및 근거

ORD 기록
ord-a662aa964a234715a1d7f3630eb82533
출처 데이터셋
uspto-grants-2006_04
특허 번호
US07022847B2

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