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Hydrochloric Acid → HCID 67976039、化合物

HRID 2046190
ノート
印刷プレビュー

反応式

HRID 2046190 の反応式
Cl[Si:2]([CH3:5])([CH3:4])[CH3:3].[OH:6][CH2:7][C@@H:8]1[CH2:13][N:12]2[N:14]=[C:15]([CH2:17][O:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH:16]=[C:11]2[C:10](=[O:25])[NH:9]1.Cl>C(#N)C>[O:18]([CH2:17][C:15]1[CH:16]=[C:11]2[C:10](=[O:25])[NH:9][C@H:8]([CH2:7][O:6][Si:2]([CH3:5])([CH3:4])[CH3:3])[CH2:13][N:12]2[N:14]=1)[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 6397ChlorotrimethylsilaneHCID 67974237(S)-6-hydroxymethyl-2-phenoxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one

生成物 1

HCID 67976039HCID 67976039、化合物収率 90%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Chlorotrimethylsilane (0.30 mL, 2.41 mmol) was added to a solution of (S)-6-hydroxymethyl-2-phenoxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one (0.33 g, 2.4 mmol) and TEA (0.33 mL, 2.4 mmol) in ACN (6 mL) at 0° C. The reaction was stirred for 30 minutes at room temperature. Then a 1N solution of HCl was added and the mixture extracted with AcOEt. The organic layer was separated, dried (Na2SO4), filtered and the solvent evaporated in vacuo to yield (S)-2-phenoxymethyl-6-trimethylsilanyloxymethyl-6,7-dihydro-5H-pyrazolo[1,5-a]pyrazin-4-one (0.375 g, 90% yield) as an off-white solid that was used in the next step without further purification.

後処理

  1. extractionthe mixture extracted with AcOEt
  2. customThe organic layer was separated
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. customthe solvent evaporated in vacuo

出典と根拠

ORDレコード
ord-b7a7132a11be4abba77b4a3b1ebdc587
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08592422B2

反応ノート

読み込み中…

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