二氯甲烷 → HCID 10631441，化合物

HRID 1069641笔记

反应方程式

HRID 1069641 反应方程式
[CH:1]1([C:4]([C:6]2[CH:11]=[C:10]([O:12][CH3:13])[CH:9]=[CH:8][C:7]=2[NH:14]C(OC(C)(C)C)=O)=O)[CH2:3][CH2:2]1.[CH2:22](Cl)Cl>FC(F)(F)C(O)=O>[CH:3]1([C:1]2[NH:14][C:7]3[C:6]([CH:4]=2)=[CH:11][C:10]([O:12][CH3:13])=[CH:9][CH:8]=3)[CH2:2][CH2:22]1

参与物

4

反应物 2

HCID 6344二氯甲烷HCID 21191890[2-(Tert-butoxycarbonylamino)-5-methoxyphenyl]cyclopropyl ketone

产物 1

HCID 10631441HCID 10631441，化合物收率 49%

试剂、催化剂与溶剂 1

HCID 6422三氟乙酸溶剂

实验过程

[2-(tert-Butoxycarbonylamino)-5-methoxyphenyl] cyclopropyl ketone (13 g, 43 mmol) in 250 mL of CH2Cl2 and 25 mL of trifluoroacetic acid was stirred for 4 hours, washed with water, NaHCO3 solution, dried (Na2SO4) and concentrated at reduced pressure. The residue was chromatographed on silica (eluted with a gradient, toluene→20% EtOAc/hexane) to give 4.15 g (49% yield) of 2-cyclopropyl-5-methoxy-1H-indole as an oil.

后处理

  1. washwashed with water, NaHCO3 solution
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated at reduced pressure
  4. customThe residue was chromatographed on silica (
  5. washeluted with a gradient, toluene

来源与证据

ORD记录
ord-961ae6e3ac4d4fdca537208760080353
来源数据集
uspto-grants-2001_06
专利号
US06252084B1

反应笔记

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