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Hydrochloric Acid → (RS)-S-(4-{[4-{[(1 R,2R)-2-Hydroxy-1-methylpropyl]amino}-5-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl)-S-methylsulfoximide

HRID 1027859
ノート
印刷プレビュー

反応式

HRID 1027859 の反応式
Cl.[NH2:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([CH3:18])(=[N:11]C(=O)C(F)(F)F)=[O:10])=[CH:5][CH:4]=1.Cl[C:20]1[N:25]=[C:24]([NH:26][C@H:27]([CH3:31])[C@H:28]([OH:30])[CH3:29])[C:23]([C:32]([F:35])([F:34])[F:33])=[CH:22][N:21]=1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.C(#N)C.[Cl-].[Na+].CO>[OH:30][C@H:28]([CH3:29])[C@H:27]([NH:26][C:24]1[C:23]([C:32]([F:35])([F:34])[F:33])=[CH:22][N:21]=[C:20]([NH:2][C:3]2[CH:4]=[CH:5][C:6]([S:9]([CH3:18])(=[NH:11])=[O:10])=[CH:7][CH:8]=2)[N:25]=1)[CH3:31]
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

9

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 58533493(RS)-S-(4-Aminophenyl)-S-methyl-N-(trifluoroacetyl)sulfoximideHCID 59683169(2R,3R)-3-(2-Chloro-5-trifluoromethylpyrimidin-4-ylamino)butan-2-ol

生成物 1

HCID 45381084(RS)-S-(4-{[4-{[(1 R,2R)-2-Hydroxy-1-methylpropyl]amino}-5-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl)-S-methylsulfoximide
収率 93.3%

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 5234Sodium Chloride溶媒HCID 6342Acetonitrile溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

0.38 ml of 4N solution of hydrogen chloride in dioxane was added to 399 mg (1.50 mmol) of (RS)-S-(4-aminophenyl)-S-methyl-N-(trifluoroacetyl)sulfoximide and 404 mg (1.50 mmol) of (2R,3R)-3-(2-chloro-5-trifluoromethyl-pyrimidin-4-ylamino)-butan-2-ol in 7.3 ml acetonitrile and stirred for 9 hours at 60° C. The mixture was evaporated to dryness. 32.2 ml methanol and 1040 mg (7.50 mmol) of potassium carbonate were added and it was stirred for 1.5 hours at room temperature. It was diluted with saturated sodium chloride solution and was extracted with ethyl acetate (3×). The combined organic phases were dried (Na2SO4), filtered and concentrated by evaporation. 565 mg (1.40 mmol) of the raw product was obtained.

後処理

  1. customThe mixture was evaporated to dryness
  2. stirringit was stirred for 1.5 hours at room temperature
  3. extractionwas extracted with ethyl acetate (3×)
  4. dry with materialThe combined organic phases were dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-5fae2db7220c44d89dace81b648f3ad5
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08735412B2

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