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Sodium Sulfate → HCID 9800992、化合物

HRID 1700122
ノート
印刷プレビュー

反応式

HRID 1700122 の反応式
[F:1][C:2]([F:38])([F:37])[C:3]1[CH:4]=[C:5]([C:9]2[N:10]=[N:11][C:12]([CH:21]3[CH2:26][CH2:25][N:24]([C:27](OCC4C=CC=CC=4)=O)[CH2:23][CH2:22]3)=[CH:13][C:14]=2[C:15]2[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=2)[CH:6]=[CH:7][CH:8]=1.[H-].[H-].[H-].[H-].[Li+].[Al+3].[O-]S([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[F:38][C:2]([F:1])([F:37])[C:3]1[CH:4]=[C:5]([C:9]2[N:10]=[N:11][C:12]([CH:21]3[CH2:22][CH2:23][N:24]([CH3:27])[CH2:25][CH2:26]3)=[CH:13][C:14]=2[C:15]2[CH:16]=[CH:17][N:18]=[CH:19][CH:20]=2)[CH:6]=[CH:7][CH:8]=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

5

反応物 3

HCID 24436Sodium SulfateHCID 18317249HCID 18317249、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 9800992HCID 9800992、化合物収率 53.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

Under Ar, a solution of 15 (0.73 g, 1.4 mmol) in THF (175 mL) was treated with LAH (0.37 g, 9.7 mmol). After addition, the reaction was heated at 60° C. After 2 h, the reaction was cooled to room temperature and treated with saturated Na2SO4 until a suspension results. The reaction mixture was filtered and the filtrate washed with EtOAc. The organic was washed with H2O, brine, dried, filtered and concentrated to dryness. The residue was treated with Et2O-hexanes, filtered and dried to yield 0.3 g of 16; mp 188-9° C.

後処理

  1. additionAfter addition
  2. temperaturethe reaction was cooled to room temperature
  3. customresults
  4. filtrationThe reaction mixture was filtered
  5. washthe filtrate washed with EtOAc
  6. washThe organic was washed with H2O, brine
  7. customdried
  8. filtrationfiltered
  9. concentrationconcentrated to dryness
  10. additionThe residue was treated with Et2O-hexanes
  11. filtrationfiltered
  12. customdried

出典と根拠

ORDレコード
ord-d023c7e0d20943dd8361aaa0c4a5a851
出典データセット
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06350744B1

反応ノート

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