Water → HCID 68731776, 화합물

HRID 1259311노트

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HRID 1259311 반응식
C(O[CH:4](OCC)[C:5]#[C:6][C:7]1[N:12]=[C:11]([C:13]([O:15][CH3:16])=[O:14])[C:10](=[O:17])[N:9]([C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([F:27])([F:26])[F:25])[CH:19]=2)[C:8]=1[CH3:28])C.Cl.[NH:33]([C:35]1[CH:42]=[CH:41][C:38]([C:39]#[N:40])=[CH:37][CH:36]=1)[NH2:34].O>CO>[C:39]([C:38]1[CH:41]=[CH:42][C:35]([NH:33][N:34]=[CH:4][C:5]#[C:6][C:7]2[N:12]=[C:11]([C:13]([O:15][CH3:16])=[O:14])[C:10](=[O:17])[N:9]([C:18]3[CH:23]=[CH:22][CH:21]=[C:20]([C:24]([F:25])([F:26])[F:27])[CH:19]=3)[C:8]=2[CH3:28])=[CH:36][CH:37]=1)#[N:40]

참가 물질

5

반응물 3

HCID 962Water2회HCID 162129624-Cyanophenylhydrazine HydrochlorideHCID 59564940Methyl 6-(3,3-diethoxyprop-1-ynyl)-5-methyl-3-oxo-4-(3-(trifluoromethyl)phenyl)-3,4-dihydropyrazine-2-carboxylate

생성물 1

HCID 68731776HCID 68731776, 화합물수율 95%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
45 °C

실험 절차

In a 100 mL round-bottomed flask, methyl 6-(3,3-diethoxyprop-1-ynyl)-5-methyl-3-oxo-4-(3-(trifluoromethyl)phenyl)-3,4-dihydropyrazine-2-carboxylate (SM2, 1.136 g, 2.59 mmol) and 4-hydrazinylbenzonitrile hydrochloride (0.508 g, 3.00 mmol) were stirred in methanol (25 mL) and water (2.5 ml) under air at 65° C. After 1 h, the mixture was allowed to cool to 45° C., water (50 ml) was added and the mixture then cooled to RT. After stirring for 30 minutes, the solid was filtered off, washed with water (100 ml) and then air dried to give methyl 6-(3-(2-(4-cyanophenyl)hydrazono)prop-1-ynyl)-5-methyl-3-oxo-4-(3-(trifluoromethyl)phenyl)-3,4-dihydropyrazine-2-carboxylate (1.18 g, 95%) as a yellow solid.

후처리

  1. customat 65° C
  2. temperaturethe mixture then cooled to RT
  3. filtrationthe solid was filtered off
  4. washwashed with water (100 ml)
  5. customair dried

출처 및 근거

ORD 기록
ord-741e31ed1aa04543ade2d05b14e35a8a
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08466284B2

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