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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Methanol → 2-{3-(4-Chlorophenyl)-5-oxo-4-[(2S)-3,3,3-trifluoro-2-hydroxypropyl]-4,5-dihydro-1H-1,2,4-triazol-1-yl}-N-{2-[(methylsulphonyl)amino]-2-[3-(trifluoromethyl)phenyl]ethyl}acetamide

HRID 709158
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HRID 709158 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].Cl.[NH2:7][CH:8]([C:34]1[CH:39]=[CH:38][CH:37]=[C:36]([C:40]([F:43])([F:42])[F:41])[CH:35]=1)[CH2:9][NH:10][C:11](=[O:33])[CH2:12][N:13]1[C:17](=[O:18])[N:16]([CH2:19][C@H:20]([OH:25])[C:21]([F:24])([F:23])[F:22])[C:15]([C:26]2[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][CH:27]=2)=[N:14]1.O.CO>N1C=CC=CC=1.CS(C)=O>[Cl:32][C:29]1[CH:30]=[CH:31][C:26]([C:15]2[N:16]([CH2:19][C@H:20]([OH:25])[C:21]([F:24])([F:22])[F:23])[C:17](=[O:18])[N:13]([CH2:12][C:11]([NH:10][CH2:9][CH:8]([NH:7][S:2]([CH3:1])(=[O:4])=[O:3])[C:34]3[CH:39]=[CH:38][CH:37]=[C:36]([C:40]([F:41])([F:42])[F:43])[CH:35]=3)=[O:33])[N:14]=2)=[CH:27][CH:28]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 887MethanolHCID 962WaterHCID 31297Methanesulfonyl chloride2회HCID 89765105N-{2-Amino-2-[3-(trifluoromethyl)phenyl]ethyl}-2-{3-(4-chlorophenyl)-5-oxo-4-[(2S)-3,3,3-trifluoro-2-hydroxypropyl]-4,5-dihydro-1H-1,2,4-triazol-1-yl}acetamide hydrochloride

생성물 1

HCID 87085250
2-{3-(4-Chlorophenyl)-5-oxo-4-[(2S)-3,3,3-trifluoro-2-hydroxypropyl]-4,5-dihydro-1H-1,2,4-triazol-1-yl}-N-{2-[(methylsulphonyl)amino]-2-[3-(trifluoromethyl)phenyl]ethyl}acetamide

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 1049Pyridine용매

실험 절차

4 μl (56 μmol) of methanesulphonyl chloride were added to a solution of 30 mg (51 μmol) of the compound of Example 58A in 0.5 ml of pyridine, and the mixture was stirred at RT overnight. Since HPLC analysis showed a lot of remaining starting material, further equivalents of methane-sulphonyl chloride (3.1 eq. in total) were added a little at a time until complete conversion had been achieved. 100 μl each of water and methanol were then added. After 5 min of stirring, the reaction mixture was diluted with about 3 ml of DMSO and separated by preparative HPLC [Method 8]. The product-containing fraction was freed from the solvent on a rotary evaporator and the residue was dried under high vacuum. This gave 22 mg (68% of theory) of the title compound.

후처리

  1. additionwere added a little at a time until complete conversion
  2. stirringAfter 5 min of stirring
  3. customseparated by preparative HPLC [Method 8]
  4. customThe product-containing fraction was freed from the solvent on a rotary evaporator
  5. customthe residue was dried under high vacuum

출처 및 근거

ORD 기록
ord-5d026a741be943ec9075dfc8f02b51a3
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09180120B2

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