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Hydrochloric Acid → HCID 178479495, 화합물

HRID 1581502
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HRID 1581502 반응식
[NH:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:25]=[CH:24][C:17]([C:18]([NH:20][C:21]([NH2:23])=[NH:22])=[O:19])=[CH:16][C:15]=2[C:26]([F:29])([F:28])[F:27])[CH2:10][CH2:9]1)=[O:7].[ClH:30]>O>[OH2:7].[ClH:30].[NH:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[CH:25]=[CH:24][C:17]([C:18]([NH:20][C:21]([NH2:23])=[NH:22])=[O:19])=[CH:16][C:15]=2[C:26]([F:28])([F:29])[F:27])[CH2:12][CH2:13]1)=[O:7]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 178513062HCID 178513062, 화합물

생성물 1

HCID 178479495HCID 178479495, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
50 °C

실험 절차

109.4 g of 4-[4-(2-pyrrolylcarbonyl)-1-piperazinyl]-3-trifluoromethylbenzoylguanidine is suspended in 1.5 L of water and heated to about 50° C. 26.1 mL of concentrated aqueous hydrochloric acid is diluted with 300 mL of water and added dropwise to the preheated suspension within about 20 minutes. The mixture is stirred for about 15 minutes at constant temperature. Then the temperature is lowered to about 35° C. with stirring over a period of about 1.5 hours. It is then cooled to 5° C. to 10° C. and stirred for another hour at this temperature. The crystals obtained are separated off, washed with a little water, and dried in vacuo at about 50° C. Yield: 116.5 g; melting point: 180° C. ±5° C. (DSC at a heating rate of 10 K/min).

후처리

  1. additionadded dropwise to the preheated suspension within about 20 minutes
  2. customis lowered to about 35° C.
  3. stirringwith stirring over a period of about 1.5 hours
  4. temperatureIt is then cooled to 5° C. to 10° C.
  5. stirringstirred for another hour at this temperature
  6. customThe crystals obtained
  7. customare separated off
  8. washwashed with a little water
  9. customdried in vacuo at about 50° C

출처 및 근거

ORD 기록
ord-a2f067a757914d9684fdfa1fb02790a3
출처 데이터셋
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06730678B2

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