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Hydrochloric Acid → HCID 67595026、化合物

HRID 865306
ノート
印刷プレビュー

反応式

HRID 865306 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:12])[CH2:7][S:8][CH2:9]2)=[CH:4][CH:3]=1.C[Si]([N-][Si](C)(C)C)(C)C.[Na+].[F:23][C:24]([F:33])([F:32])[C:25](C1NC=CN=1)=[O:26].Cl>O1CCCC1>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:12])[CH:7]([C:25](=[O:26])[C:24]([F:33])([F:32])[F:23])[S:8][CH2:9]2)=[CH:4][CH:3]=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

6

反応物 4

HCID 313Hydrochloric AcidHCID 5654362,2,2-Trifluoro-1-(1H-imidazol-2-yl)ethanoneHCID 2724254Sodium bis(trimethylsilyl)amideHCID 22394204HCID 22394204、化合物

生成物 1

HCID 67595026HCID 67595026、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-78 °C

実験手順

7-Chloroisothiochroman-4-one from Step 3 (0.3 g, 1.5 mmol) was dissolved in tetrahydrofuran (15 mL) and cooled to -78° C. A solution of sodium bistrimethylsilyl amide (1.5 mL of a 1.0M tetrahydrofuran solution) was added and the reaction stirred for 0.5 hours at -78° C. Trifluoroacetyl imidazole (0.21 mL, 1.8 mmol) was added and the reaction was warmed to room temperature and stirred under a nitrogen atmosphere for 16 hours. 1N Hydrochloric acid (100 mL) was added to the reaction followed by extraction with ether (150 mL). The organics were washed with brine (75 mL), dried over MgSO4 and concentrated in vacuo. The resulting yellow oil was used in the next step without further purification.

後処理

  1. temperaturethe reaction was warmed to room temperature
  2. stirringstirred under a nitrogen atmosphere for 16 hours
  3. extractionfollowed by extraction with ether (150 mL)
  4. washThe organics were washed with brine (75 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. customThe resulting yellow oil was used in the next step without further purification

出典と根拠

ORDレコード
ord-f1a09d8bb4fb4ff58a34adc267418e3b
出典データセット
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05565482

反応ノート

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