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1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride → HCID 11613717、化合物

HRID 1713999
ノート
印刷プレビュー

反応式

HRID 1713999 の反応式
Cl.C(N=C=NCCCN(C)C)C.[CH3:13][O:14][C:15](=[O:21])[CH2:16][S:17]([NH2:20])(=[O:19])=[O:18].[CH:22]1([C:28]2[C:29]3[CH:30]=[CH:31][C:32]([C:50](O)=[O:51])=[CH:33][C:34]=3[N:35]3[CH2:42][CH2:41][N:40]([CH3:43])[CH2:39][C:38]4[CH:44]=[C:45]([O:48][CH3:49])[CH:46]=[CH:47][C:37]=4[C:36]=23)[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1>CN(C1C=CN=CC=1)C.C(Cl)Cl>[CH3:13][O:14][C:15](=[O:21])[CH2:16][S:17]([NH:20][C:50]([C:32]1[CH:31]=[CH:30][C:29]2[C:28]([CH:22]3[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]3)=[C:36]3[C:37]4[CH:47]=[CH:46][C:45]([O:48][CH3:49])=[CH:44][C:38]=4[CH2:39][N:40]([CH3:43])[CH2:41][CH2:42][N:35]3[C:34]=2[CH:33]=1)=[O:51])(=[O:19])=[O:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 21287077Methyl 2-sulfamoylacetateHCID 42640442HCID 42640442、化合物

生成物 1

HCID 11613717HCID 11613717、化合物収率 18%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒
HCID 6344
Dichloromethane
溶媒

実験手順

1.6 eq of 1-ethyl-(3-dimethylaminopropyl)carbodiimide HCl salt was added to a mixture of 2.7 eq of DMAP, 1.6 eq of methyl(aminosulfonyl)acetate and the hydrochloride salt of 14-cyclohexyl-3-methoxy-6-methyl-5,6,7,8-tetrahydroindolo[2,1-a][2,5]-benzodiazocine-11-carboxylic acid (from Example 4) in DCM (0.02 M). The reaction was stirred at RT overnight before being partitioned between aqueous HCl (1 N) and EtOAc. The organics were washed with saturated aqueous NaHCO3, water and brine before being dried over Na2SO4, filtered and concentrated in vacuo. The crude was then purified by RP-HPLC (stationary phase: column Waters XTERRA prep. C18, 5 um, 30×50 mm. Mobile phase: MeCN/H2O buffered with 0.1% TFA). Fractions containing the pure compound were combined and freeze dried to afford the title compound as a white powder (18%).

後処理

  1. custombefore being partitioned between aqueous HCl (1 N) and EtOAc
  2. washThe organics were washed with saturated aqueous NaHCO3, water and brine
  3. dry with materialbefore being dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude was then purified by RP-HPLC (stationary phase: column Waters XTERRA prep. C18, 5 um, 30×50 mm. Mobile phase: MeCN/H2O buffered with 0.1% TFA)
  7. additionFractions containing the pure compound
  8. customfreeze dried

出典と根拠

ORDレコード
ord-3ff17dbf438849369a2d81b324d52baa
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07795247B2

反応ノート

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