Hydrochloric Acid → HCID 178449906、化合物

HRID 1794584ノート

反応式

HRID 1794584 の反応式
[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]

参加物

7

反応物 5

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

生成物 1

HCID 178449906HCID 178449906、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a662aa964a234715a1d7f3630eb82533
出典データセット
uspto-grants-2006_04
特許番号
US07022847B2

反応ノート

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