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Hydrochloric Acid → 4-(3-Cyclopentyl-indole-1-sulfonyl)-N-(tetrahydro-pyran-4-ylmethyl)-benzamide

HRID 737048
ノート
印刷プレビュー

反応式

HRID 737048 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][CH2:46][CH:47]1[CH2:52][CH2:51][O:50][CH2:49][CH2:48]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][CH2:46][CH:47]4[CH2:52][CH2:51][O:50][CH2:49][CH2:48]4)=[O:24])=[CH:20][CH:19]=3)(=[O:16])=[O:17])[CH:7]=2)[CH2:2][CH2:3][CH2:4][CH2:5]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 27732104-AminomethyltetrahydropyranHCID 58975136HCID 58975136、化合物

生成物 1

HCID 112021584-(3-Cyclopentyl-indole-1-sulfonyl)-N-(tetrahydro-pyran-4-ylmethyl)-benzamide

試薬・触媒・溶媒

2
HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
5 °C

実験手順

Stir a stir 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. under N2 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 for 1 h and add a solution of 4-aminomethyltetrahydropyran (6.6 g, 57.34 mmol) in dry THF (75 mL) by dropping funnel. Warm the mixture to room temperature and stir for 3 h. Cool the mixture to 5° C., add 1N HCl (250 mL) and partition the resulting solution with ethyl acetate (250 mL). Extract the organic layer with aqueous saturated sodium bicarbonate (250 mL), brine (250 mL), and dry over sodium sulfate. Concentrate to give a foam, dissolve in minimum methylene chloride and add to a flash 65 M cartridge. Elute with 3:2 hexanes/ethyl acetate to give the major product as a solid, filter from hexanes, and dry (20 mm Hg, 40° C.) to give the homogeneous white solid (20.5 g, 85%); MS (ESI) m/z 467 (m+H).

後処理

  1. temperatureWarm the mixture to room temperature
  2. stirringstir for 3 h
  3. temperatureCool the mixture to 5° C.
  4. custompartition the resulting solution with ethyl acetate (250 mL)
  5. extractionExtract the organic layer with aqueous saturated sodium bicarbonate (250 mL), brine (250 mL)
  6. dry with materialdry over sodium sulfate
  7. concentrationConcentrate
  8. customto give a foam
  9. additionadd to a flash 65 M cartridge
  10. washElute with 3:2 hexanes/ethyl acetate

出典と根拠

ORDレコード
ord-9308f3f7aa474b81a8674b5fa7501877
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07595339B2

反応ノート

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