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1-Hydroxybenzotriazole → HCID 58012169、化合物

HRID 660906
ノート
印刷プレビュー

反応式

HRID 660906 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:9][C:10](=[O:17])[N:11]([CH2:13][C:14]([OH:16])=O)[CH:12]=2)=[CH:4][CH:3]=1.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl.[F:40][C:41]([F:53])([F:52])[C:42]1[CH:43]=[C:44]([C:48]([NH2:51])([CH3:50])[CH3:49])[CH:45]=[CH:46][CH:47]=1>CN(C=O)C.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[NH:9][C:10](=[O:17])[N:11]([CH2:13][C:14]([NH:51][C:48]([CH3:50])([C:44]3[CH:45]=[CH:46][CH:47]=[C:42]([C:41]([F:40])([F:52])[F:53])[CH:43]=3)[CH3:49])=[O:16])[CH:12]=2)=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 194252732-[3-(Trifluoromethyl)phenyl]propan-2-amineHCID 58011978HCID 58011978、化合物

生成物 1

HCID 58012169HCID 58012169、化合物

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

318 mg (1.26 mmol) of [4-(4-chlorophenyl)-2-oxo-2,3-dihydro-1H-imidazol-1-yl]-acetic acid from Example 233A are placed in 10 ml DMF and treated with 221 mg (1.64 mmol) of HOBt and 314 mg (1.64 mmol) of EDC hydrochloride. After 10 mins' stirring, 332 mg (1.64 mmol) of 1-methyl-1-[(3-trifluoromethyl)phenyl]ethylamine from Example 1A are added and the mixture is stirred overnight at room temperature. For the workup, the reaction mixture is stirred with 100 ml water. Next, the resulting precipitate is suction-filtered, washed with water and dried under high vacuum. Further purification is effected by preparative HPLC [Method 10]. 209 mg (38% of theory) of the target compound are thus obtained.

後処理

  1. stirringthe mixture is stirred overnight at room temperature
  2. filtrationNext, the resulting precipitate is suction-filtered
  3. washwashed with water
  4. customdried under high vacuum
  5. customFurther purification
  6. custom209 mg (38% of theory) of the target compound are thus obtained

出典と根拠

ORDレコード
ord-3f3a987169e14c18a32a7c1498736b38
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084481B2

反応ノート

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