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Hydrochloric Acid → HCID 66955253、化合物

HRID 1948532
ノート
印刷プレビュー

反応式

HRID 1948532 の反応式
C([C:3]1([O:16][Si:17]([CH3:20])([CH3:19])[CH3:18])[CH2:8][CH2:7][CH2:6][N:5](C(OC(C)(C)C)=O)[CH2:4]1)#N.Cl.[C:22](=[O:25])([O-])[O-:23].[Cs+].[Cs+].[Si](Cl)(C)(C)[CH3:29]>CO>[CH3:18][Si:17]([CH3:19])([CH3:20])[O:16][C:3]1([C:22]([O:23][CH3:29])=[O:25])[CH2:8][CH2:7][CH2:6][NH:5][CH2:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6397ChlorotrimethylsilaneHCID 10796Cesium carbonateHCID 58374194Tert-butyl 3-cyano-3-(trimethylsilyloxy)piperidine-1-carboxylate

生成物 1

HCID 66955253HCID 66955253、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

tert-Butyl 3-cyano-3-(trimethylsilyloxy)piperidine-1-carboxylate, Preparation 34A (170 mg, 0.570 mmol) was treated with 6N HCl in MeOH (10 mL) at 80° C. for 12 hours. Solvents were removed in vacuo and the resulting material was dissolved in MeOH (10 mL). HCl (g) was bubbled through the mixture for 15 minutes. The solids were concentrated in vacuo. The residue was dissolved in DCM (10.00 mL) and cesium carbonate (928 mg, 2.85 mmol) was added. Next, TMS—Cl (0.146 mL, 1.139 mmol) was added and the mixture was stirred for 1 hour. The mixture was filtered and the solids were concentrated in vacuo and taken to the next step without further purification.

後処理

  1. customSolvents were removed in vacuo
  2. dissolutionthe resulting material was dissolved in MeOH (10 mL)
  3. customHCl (g) was bubbled through the mixture for 15 minutes
  4. concentrationThe solids were concentrated in vacuo
  5. dissolutionThe residue was dissolved in DCM (10.00 mL)
  6. filtrationThe mixture was filtered
  7. concentrationthe solids were concentrated in vacuo
  8. customtaken to the next step without further purification

出典と根拠

ORDレコード
ord-5e18151ba7b7423fb6a52dcf8095f488
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399451B2

反応ノート

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