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(Diethylamino)sulfur trifluoride → HCID 59389401、化合物

HRID 2357923
ノート
印刷プレビュー

反応式

HRID 2357923 の反応式
CCN(S(F)(F)[F:7])CC.O[CH:11]([C:13]1[CH:31]=[C:16]2[C:17]([C:23]3[CH:24]([CH3:30])[CH2:25][C:26](=[O:29])[NH:27][N:28]=3)=[CH:18][CH:19]=[C:20]([O:21][CH3:22])[N:15]2[N:14]=1)[CH3:12]>C(Cl)(Cl)Cl>[F:7][CH:11]([C:13]1[CH:31]=[C:16]2[C:17]([C:23]3[CH:24]([CH3:30])[CH2:25][C:26](=[O:29])[NH:27][N:28]=3)=[CH:18][CH:19]=[C:20]([O:21][CH3:22])[N:15]2[N:14]=1)[CH3:12]
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

4

反応物 2

HCID 123472(Diethylamino)sulfur trifluorideHCID 59389404HCID 59389404、化合物

生成物 1

HCID 59389401HCID 59389401、化合物収率 38%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
0 °C

実験手順

DAST (51.2 mg) was added dropwise to a solution of the compound of Example 238 (80.0 mg) in chloroform (10 mL) at 0° C. and the mixture was stirred at 0° C. for 30 min. The reaction was quenched by adding a saturated aqueous sodium bicarbonate solution and the reaction mixture was extracted with chloroform (30 mL). The extract was washed with water and saturated brine and dried over anhydrous sodium sulfate. The dried extract was concentrated and purified by silica gel column chromatography (hexane:ethyl acetate=1:4) to afford the title compound as a pale yellow powder (30.6 mg).

後処理

  1. customThe reaction was quenched
  2. additionby adding a saturated aqueous sodium bicarbonate solution
  3. extractionthe reaction mixture was extracted with chloroform (30 mL)
  4. washThe extract was washed with water and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. extractionThe dried extract
  7. concentrationwas concentrated
  8. custompurified by silica gel column chromatography (hexane:ethyl acetate=1:4)

出典と根拠

ORDレコード
ord-01d097344a4341919b3951c49ca0263a
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07763617B2

反応ノート

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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