Methane → 2-[4-(4-Trifluoromethylbenzyloxy)-2-picolylmercapto]-1H-thieno[3,4-d]imidazole

HRID 1196625노트

반응식

HRID 1196625 반응식
Cl.Cl.[F:3][C:4]([F:30])([F:29])[C:5]1[CH:28]=[CH:27][C:8]([CH2:9][O:10][C:11]2[CH:16]=[CH:15][N:14]=[C:13]([CH2:17][S:18][C:19]3[NH:23][C:22]4=[CH:24][S:25][CH:26]=[C:21]4[N:20]=3)[CH:12]=2)=[CH:7][CH:6]=1.C(N(CC)CC)C.C>CO>[F:30][C:4]([F:3])([F:29])[C:5]1[CH:28]=[CH:27][C:8]([CH2:9][O:10][C:11]2[CH:16]=[CH:15][N:14]=[C:13]([CH2:17][S:18][C:19]3[NH:23][C:22]4=[CH:24][S:25][CH:26]=[C:21]4[N:20]=3)[CH:12]=2)=[CH:7][CH:6]=1

참가 물질

5

반응물 3

HCID 297MethaneHCID 8471TriethylamineHCID 198989772-[4-(4-Trifluoromethylbenzyloxy)-2-picolylmercapto]-1H-thieno[3,4-d]imidazole dihydrochloride

생성물 1

HCID 144259992-[4-(4-Trifluoromethylbenzyloxy)-2-picolylmercapto]-1H-thieno[3,4-d]imidazole

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1.5 g (3.0 mmol) of the dihydrochloride from Example 5 are suspended in 25 ml of methanol with ice-cooling and under a nitrogen atmosphere and 1.7 ml (about 12 mmol) of triethylamine are added dropwise, by means of which a clear solution is formed which is subsequently clarified over activated charcoal and concentrated. On treating with water, the residue crystallizes and is washed with water and dried in vacuo, m.p. 141°-143° C. with decomposition.

후처리

  1. temperaturecooling and under a nitrogen atmosphere
  2. customis formed which
  3. concentrationconcentrated
  4. additionOn treating with water
  5. customthe residue crystallizes
  6. washis washed with water
  7. customdried in vacuo, m.p. 141°-143° C. with decomposition

출처 및 근거

ORD 기록
ord-4cf7b20f667542b8a11deb620439097e
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05114955

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