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Diisopropylethylamine → 3-benzyloxy-N-(5-tert-butyl-3-methanesulphonylamino-2-methoxy-phenyl)-4-methyl-benzamide

HRID 1844590
ノート
印刷プレビュー

反応式

HRID 1844590 の反応式
F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.C(N(C(C)C)CC)(C)C.ON1C2N=CC=CC=2N=N1.[CH2:44]([O:51][C:52]1[CH:53]=[C:54]([CH:58]=[CH:59][C:60]=1[CH3:61])[C:55]([OH:57])=O)[C:45]1[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=1.Cl.[NH2:63][C:64]1[C:65]([O:79][CH3:80])=[C:66]([NH:74][S:75]([CH3:78])(=[O:77])=[O:76])[CH:67]=[C:68]([C:70]([CH3:73])([CH3:72])[CH3:71])[CH:69]=1>CN(C)C=O.C(OCC)(=O)C>[CH2:44]([O:51][C:52]1[CH:53]=[C:54]([CH:58]=[CH:59][C:60]=1[CH3:61])[C:55]([NH:63][C:64]1[CH:69]=[C:68]([C:70]([CH3:72])([CH3:73])[CH3:71])[CH:67]=[C:66]([NH:74][S:75]([CH3:78])(=[O:77])=[O:76])[C:65]=1[O:79][CH3:80])=[O:57])[C:45]1[CH:46]=[CH:47][CH:48]=[CH:49][CH:50]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 81531DiisopropylethylamineHCID 181649HOAtHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 21079205N-(3-amino-5-tert-butyl-2-methoxyphenyl)methanesulphonamide-hydrochlorideHCID 229031883-(Benzyloxy)-4-methylbenzoic acid

生成物 1

HCID 67217548
3-benzyloxy-N-(5-tert-butyl-3-methanesulphonylamino-2-methoxy-phenyl)-4-methyl-benzamide

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

10.59 g of O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyl-uronium hexafluorophosphate, 9.54 ml diisopropylethylamine and 1.26 g 1-hydroxy-7-azabenzotriazole are added to 4.50 g 3-benzyloxy-4-methyl-benzoic acid in 25 ml N,N-dimethylformamide under an argon atmosphere. The mixture is stirred for 15 minutes at ambient temperature, before 5.74 g N-(3-amino-5-tert-butyl-2-methoxyphenyl)methanesulphonamide-hydrochloride are added. The reaction mixture is stirred overnight at 50° C. After cooling to ambient temperature the reaction mixture is diluted with ethyl acetate, washed with water, 1 N hydrochloric acid and saturated aqueous sodium chloride solution, dried on magnesium sulphate and evaporated down. The flask residue is stirred with methanol, and the resulting white precipitate is suction filtered and dried.

後処理

  1. additionare added
  2. temperatureAfter cooling to ambient temperature the reaction mixture
  3. washwashed with water, 1 N hydrochloric acid and saturated aqueous sodium chloride solution
  4. customdried on magnesium sulphate
  5. customevaporated down
  6. stirringThe flask residue is stirred with methanol
  7. filtrationfiltered
  8. customdried

出典と根拠

ORDレコード
ord-0ef8f2f3e5bb4b97af5414d0a35b9125
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946438B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート