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Hydrochloric Acid → HCID 11247975、化合物

HRID 1178982
ノート
印刷プレビュー

反応式

HRID 1178982 の反応式
[CH:1]1([C:6]2[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[N:8]([S:15]([C:18]3[CH:26]=[CH:25][C:21]([C:22]([OH:24])=O)=[CH:20][CH:19]=3)(=[O:17])=[O:16])[CH:7]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.CN1CCOCC1.ClC1N=C(OC)N=C(OC)N=1.[NH2:45][CH:46]1[CH2:51][CH2:50][O:49][CH2:48][CH2:47]1.Cl>C1COCC1.C(Cl)Cl>[CH:1]1([C:6]2[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[N:8]([S:15]([C:18]3[CH:26]=[CH:25][C:21]([C:22]([NH:45][CH:46]4[CH2:51][CH2:50][O:49][CH2:48][CH2:47]4)=[O:24])=[CH:20][CH:19]=3)(=[O:17])=[O:16])[CH:7]=2)[CH2:5][CH2:4][CH2:3][CH2:2]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

8

反応物 5

HCID 313Hydrochloric AcidHCID 79724-MethylmorpholineHCID 184502-Chloro-4,6-dimethoxy-1,3,5-triazineHCID 4192234-AminotetrahydropyranHCID 58975136HCID 58975136、化合物

生成物 1

HCID 11247975HCID 11247975、化合物

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
5 °C

実験手順

Stir a solution of 4-(3-cyclopentyl-indole-1-sulfonyl)-benzoic acid (19.0 g, 51.43 mmol) in anhydrous THF (250 mL), cool to 5° C., add N-methylmorpholine (5.8 mL, 52.72 mmol) and 2-chloro-4,6-dimethoxy-1,3,5-triazine (CDMT) (9.0 g, 51.34 mmol). Stir the mixture at 0-5° C. for 1 h, add a solution of 4-aminotetrahydro-pyran (5.8 g, 57.36 mmol) in dry THF (75 mL) via dropping funnel. Bring the mixture to room temperature, stir for 3 h, and cool back down to 5° C. Stir the mixture and add 1N HCl (250 mL), add the resulting solution to a separatory funnel, and extract with ethyl acetate (250 mL). Separate the layers, wash the organic layer with brine (250 mL), and combine the aqueous layers and extract with ethyl acetate (250 mL). Combine the organics and wash with saturated aqueous sodium bicarbonate (400 mL) and dry the organic layer over sodium sulfate. Concentrate to give a foam, dissolve in minimum methylene chloride, and add to a biotage flash 65M cartridge. Elute with 3:2 hexanes/ethyl acetate to provide the major product as a foam, and dry (20 mm Hg, 40° C.) to give a white powder of pure product (20.3 g, 87%); MS (ESI) m/z 453 (m+H).

後処理

  1. stirringBring the mixture to room temperature, stir for 3 h
  2. temperaturecool back down to 5° C
  3. stirringStir the mixture
  4. additionadd the resulting solution to a separatory funnel
  5. extractionextract with ethyl acetate (250 mL)
  6. customSeparate the layers
  7. washwash the organic layer with brine (250 mL)
  8. extractionextract with ethyl acetate (250 mL)
  9. washCombine the organics and wash with saturated aqueous sodium bicarbonate (400 mL)
  10. dry with materialdry the organic layer over sodium sulfate
  11. concentrationConcentrate
  12. customto give a foam
  13. additionadd to a biotage flash 65M cartridge
  14. washElute with 3:2 hexanes/ethyl acetate

出典と根拠

ORDレコード
ord-3afe47aa07394d42baf708b8e6e132e3
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07276516B2

反応ノート

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