Trifluoroacetic acid → HCID 24960733、化合物

HRID 1662830ノート

反応式

HRID 1662830 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:20])[C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=2)=[CH:7][C:3]=1[C:4]([OH:6])=O.ClC1N=C(OC)N=C(OC)N=1.CN1CCOCC1.C(OC([N:46]1[CH2:51][CH2:50][CH:49]([S:52]([C:55]2[CH:60]=[CH:59][C:58]([NH:61][C:62]3[N:67]=[CH:66][C:65]([NH2:68])=[CH:64][N:63]=3)=[CH:57][CH:56]=2)(=[O:54])=[O:53])[CH2:48][CH2:47]1)=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:20])[C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=2)=[CH:7][C:3]=1[C:4]([NH:68][C:65]1[CH:66]=[N:67][C:62]([NH:61][C:58]2[CH:59]=[CH:60][C:55]([S:52]([CH:49]3[CH2:50][CH2:51][NH:46][CH2:47][CH2:48]3)(=[O:53])=[O:54])=[CH:56][CH:57]=2)=[N:63][CH:64]=1)=[O:6]

参加物

7

反応物 5

HCID 6422Trifluoroacetic acidHCID 79724-MethylmorpholineHCID 184502-Chloro-4,6-dimethoxy-1,3,5-triazineHCID 28667434HCID 28667434、化合物HCID 587487264-(4-(5-Amino-pyrimidin-2-ylamino)-benzenesulfonyl)-piperidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 24960733HCID 24960733、化合物収率 11%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Intermediate 19 (Example 27) (0.136 g, 0.44 mmol) was combined with 2-chloro-4,6-dimethoxy-1,3,5-triazine (CDMT) (0.093 g, 0.53 mmol) and diluted with DCM (4 mL). This was immediately treated with 4-methyl morpholine (0.10 mL, 0.88 mmol) and allowed to stir at ambient temperature for 1 h. Intermediate 13 (Example 20) (0.20 g, 0.462 mmol) was then added in one portion. Stirring was continued overnight. After 18 h, reaction solvents were removed and resulting crude solids were diluted with DCM (4 mL) and treated with TFA (0.2 mL). After 2 h, reaction solvents were removed and resulting crude solids purified via HPLC to afford the title compound as a white solid (0.030 g, 11%).

後処理

  1. stirringStirring
  2. waitwas continued overnight
  3. waitAfter 18 h
  4. customreaction solvents
  5. customwere removed
  6. customresulting crude solids
  7. waitAfter 2 h
  8. customreaction solvents
  9. customwere removed
  10. customresulting crude solids
  11. custompurified via HPLC

出典と根拠

ORDレコード
ord-3ae72a55c64048bf9cc57e79b876d18b
出典データセット
uspto-grants-2011_10
特許番号
US08030487B2

反応ノート

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