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Hydrochloric Acid → (S)-tert-butyl 3-(((4-amino-2,2-dioxido-1H-benzo[c][1,2,6]thiadiazin-5-yl)oxy)methyl)piperidine-1-carboxylate

HRID 332945
ノート
印刷プレビュー

反応式

HRID 332945 の反応式
[NH2:1][C:2]1[C:3]([C:23]#[N:24])=[C:4]([CH:20]=[CH:21][CH:22]=1)[O:5][CH2:6][C@H:7]1[CH2:12][CH2:11][CH2:10][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:8]1.N1C=CC=CC=1.[S:31](Cl)(=[O:34])(=[O:33])[NH2:32].C([O-])(O)=O.[Na+].[OH-].[Na+].Cl>CC(N(C)C)=O.CCO.O>[NH2:24][C:23]1[C:3]2[C:4]([O:5][CH2:6][C@H:7]3[CH2:12][CH2:11][CH2:10][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:17])[CH3:18])=[O:14])[CH2:8]3)=[CH:20][CH:21]=[CH:22][C:2]=2[NH:1][S:31](=[O:34])(=[O:33])[N:32]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 6

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 14798Sodium HydroxideHCID 24499Chlorosulfamic acidHCID 516892Sodium BicarbonateHCID 86714276(S)-tert-butyl 3-((3-amino-2-cyanophenoxy)methyl)piperidine-1-carboxylate

生成物 1

HCID 86714275
(S)-tert-butyl 3-(((4-amino-2,2-dioxido-1H-benzo[c][1,2,6]thiadiazin-5-yl)oxy)methyl)piperidine-1-carboxylate

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 31374Dimethylacetamide溶媒

実験手順

To a solution of (S)-tert-butyl 3-((3-amino-2-cyanophenoxy)methyl)piperidine-1-carboxylate (Example 2c, 11.0 g, 33.2 mmol) in DMA (100 mL) was added pyridine (13.4 mL, 166 mmol) and sulfamoyl chloride (7.64 g, 66.4 mmol) in small portions. The mixture was stirred at room temperature under nitrogen for 1 hour until the reaction was complete according to LCMS. Saturated NaHCO3 was added until the mixture was neutral and the solution was extracted with EtOAc (3×). The combined organics were dried over Na2SO4 and concentrated. The residue was diluted with EtOH (100 mL) and NaOH (66.4 mL, 132.8 mmol, 2M solution) was added and the solution was heated to 80° C. for 3 hours. The reaction mixture was then allowed to cool to room temperature. The solution was further cool to 0° C. and neutralized with 2N HCl. Water was added and the desired product crashed out. The product was then filtered off and dried to yield the title compound (7.0 g, 51.4%). (M+H)-Boc=311.

後処理

  1. extractionthe solution was extracted with EtOAc (3×)
  2. dry with materialThe combined organics were dried over Na2SO4
  3. concentrationconcentrated
  4. additionwas added
  5. temperaturethe solution was heated to 80° C. for 3 hours
  6. temperatureto cool to room temperature

出典と根拠

ORDレコード
ord-d172f89c45874f0487280f5f8af07f3b
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877922B2

反応ノート

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