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Hydroxylamine → HCID 11705851、化合物

HRID 1723816
ノート
印刷プレビュー

反応式

HRID 1723816 の反応式
[CH3:1][S:2]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][C:14]([O:17][CH2:18][C:19]([F:22])([F:21])[F:20])=[CH:13][N:12]=2)[CH2:7][CH2:6]1)(=[O:4])=[O:3].[Li+].C[Si]([N-:28][Si](C)(C)C)(C)C.P(Cl)(OCC)(OCC)=O.[N:42]1[CH:47]=[CH:46][CH:45]=[CH:44][C:43]=1[CH2:48][CH2:49]C=O.[NH2:52][OH:53]>C1COCC1>[OH:53][NH:52][CH:49]([CH2:1][S:2]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][C:14]([O:17][CH2:18][C:19]([F:22])([F:20])[F:21])=[CH:13][N:12]=2)[CH2:7][CH2:6]1)(=[O:4])=[O:3])[CH2:48][CH2:43][C:42]1[N:47]=[CH:46][CH:45]=[CH:44][N:28]=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

7

反応物 5

HCID 787HydroxylamineHCID 13139Diethyl chlorophosphateHCID 2733832Lithium hexamethyldisilazaneHCID 114007983-(Pyridin-2-YL)propanalHCID 575592331-(Methanesulfonyl)-4-[5-(2,2,2-trifluoroethoxy)pyridin-2-yl]piperazine

生成物 1

HCID 11705851HCID 11705851、化合物収率 95%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

反応条件

温度
0 °C

実験手順

To a stirred suspension 1-(methylsulfonyl)-4-[5-(2,2,2-trifluoroethoxy)pyridin-2-yl]piperazine (23 g, 67.8 mmol, prepared as above) in THF (450 mL) at −65° C., was added drop wise a solution of LiHMDS in THF (149 mL, 1.0M solution, 149 mmol). Stirred for 30 minutes. Added diethyl chlorophosphate (11.3 mL, 78 mmol) and stirred for 1 hour. The solution was treated drop wise with a solution of 3-(2-pyridinyl)propaldehyde (12 g, 88.1 mmol) in THF (290 mL) and then allowed to warm to 0° C. over 3 hours before being quenched with a solution of hydroxylamine (41 mL, 50% aqueous solution in water, 680 mmol). The reaction was stirred for 16 hours at RT. The reaction washed with sat. NH4Cl (250 mL) back-extracting with ethyl acetate (250 mL). The combined organic extracts were then dried (brine and MgSO4), filtered and concentrated in vacuo. The residue was then triturated with ether for 1 hour, filtered and dried to give 2-[3-(hydroxyamino)-4-({4-[5-(2,2,2-trifluoroethoxy)pyridin-2-yl]piperazin-1-yl}sulfonyl)butyl]pyrimidine (31.5 g, 64.3 mmol, 95%).

後処理

  1. stirringThe reaction was stirred for 16 hours at RT
  2. washThe reaction washed with sat. NH4Cl (250 mL)
  3. extractionback-extracting with ethyl acetate (250 mL)
  4. dry with materialThe combined organic extracts were then dried (brine and MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was then triturated with ether for 1 hour
  8. filtrationfiltered
  9. customdried

出典と根拠

ORDレコード
ord-dccfc69233404a4db435fef5cd57141b
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07485644B2

反応ノート

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