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1-Hydroxybenzotriazole → HCID 58012169, 화합물

HRID 660906
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HRID 660906 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

HCID 58012169HCID 58012169, 화합물

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3f3a987169e14c18a32a7c1498736b38
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084481B2

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