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

HRID 1196625ノート

反応式

HRID 1196625 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4cf7b20f667542b8a11deb620439097e
出典データセット
uspto-grants-1992_05
特許番号
US05114955

反応ノート

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