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三乙胺 → HCID 178488310,化合物

HRID 1663263
笔记
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反应方程式

HRID 1663263 反应方程式
[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([N:12]2[CH:25]([CH2:26][C:27]([OH:29])=O)[C:24]3[C:19](=[C:20]([O:30][CH3:31])[CH:21]=[CH:22][CH:23]=3)[C:18]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]2=3)(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[Cl:8].C(N(CC)CC)C.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.Cl.Cl.[N:65]1([CH2:70][CH2:71][C@H:72]2[CH2:77][CH2:76][C@H:75]([NH2:78])[CH2:74][CH2:73]2)[CH2:69][CH2:68][CH2:67][CH2:66]1>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([N:12]2[CH:25]([CH2:26][C:27]([NH:78][C@H:75]3[CH2:76][CH2:77][C@H:72]([CH2:71][CH2:70][N:65]4[CH2:69][CH2:68][CH2:67][CH2:66]4)[CH2:73][CH2:74]3)=[O:29])[C:24]3[C:19](=[C:20]([O:30][CH3:31])[CH:21]=[CH:22][CH:23]=3)[C:18]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]2=3)(=[O:10])=[O:11])[CH:5]=[CH:6][C:7]=1[Cl:8]
参与物实验过程后处理来源与证据反应笔记

参与物

6

反应物 4

HCID 8471三乙胺2 次HCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 67436621HCID 67436621,化合物HCID 178478709HCID 178478709,化合物

产物 1

HCID 178488310HCID 178488310,化合物收率 60.5%

试剂、催化剂与溶剂 1

HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

A solution of [5-(3,4-dichloro-benzenesulfonyl)-10-methoxy-5,6-dihydro-phenanthridin-6-yl]-acetic acid (Example 17/d) (0.163 g, 0.34 mmol), triethylamine (0.3 mL, 2.1 mmol) and O-benzotriazol-1-yl-N,N,N′,N′-tetramethyluronium hexafluorophosphate (HBTU) (0.152 g, 0.4 mmol) in dry dimethyl formamide (10 mL) was stirred at room temperature for five minutes before trans-4-(2-pyrrolidin-1-yl-ethyl)-cyclohexylamine dihydrochloride (Reference Example 4) (0.09 g, 0.34 mmol) was added. The pH of the reaction mixture was adjusted to 8 by addition of triethylamine, the so obtained mixture was stirred at room temperature overnight, then concentrated in vacuo. The residue was treated with saturated sodium hydrogencarbonate solution (30 mL), the precipitated crystals were filtered off, washed with water and dried. The crude product was purified by column chromatography using Kieselgel 60 (0.040-0.063 mm) (Merck) as adsorbent, and chloroform:methanol:NH4OH=9:1:0.1 as eluent. The product was crystallized with diethyl ether to yield 0.135 g (60%) of the title compound. MS (EI) 657.2 (MH+).

后处理

  1. additionwas added
  2. concentrationconcentrated in vacuo
  3. additionThe residue was treated with saturated sodium hydrogencarbonate solution (30 mL)
  4. filtrationthe precipitated crystals were filtered off
  5. washwashed with water
  6. customdried
  7. customThe crude product was purified by column chromatography
  8. customThe product was crystallized with diethyl ether

来源与证据

ORD记录
ord-e69ac7d8cb804e49ad1111639474146c
来源数据集
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08034827B2

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记