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Triethylamine → (S)-methyl 4-(1-(5-chloro-2-(3-(4-fluorophenoxy)azetidin-1-yl)nicotinamido)ethyl)benzoate

HRID 72490
ノート
印刷プレビュー

反応式

HRID 72490 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][C:5]([N:11]2[CH2:14][CH:13]([O:15][C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=3)[CH2:12]2)=[C:6]([CH:10]=1)[C:7](O)=[O:8].Cl.C(N=C=NCCCN(C)C)C.Cl.[NH2:36][C@H:37]([C:39]1[CH:48]=[CH:47][C:42]([C:43]([O:45][CH3:46])=[O:44])=[CH:41][CH:40]=1)[CH3:38].C(N(CC)CC)C.C([O-])(O)=O.[Na+]>ClCCl>[Cl:1][C:2]1[CH:3]=[N:4][C:5]([N:11]2[CH2:12][CH:13]([O:15][C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][CH:17]=3)[CH2:14]2)=[C:6]([CH:10]=1)[C:7]([NH:36][C@H:37]([C:39]1[CH:48]=[CH:47][C:42]([C:43]([O:45][CH3:46])=[O:44])=[CH:41][CH:40]=1)[CH3:38])=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 57462942(S)-Methyl 4-(1-aminoethyl)benzoate hydrochlorideHCID 679580475-Chloro-2-(3-(4-fluorophenoxy)azetidin-1-yl)nicotinic acid

生成物 1

HCID 67958252
(S)-methyl 4-(1-(5-chloro-2-(3-(4-fluorophenoxy)azetidin-1-yl)nicotinamido)ethyl)benzoate
収率 89.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A mixture of 5-chloro-2-(3-(4-fluorophenoxy)azetidin-1-yl)nicotinic acid (D102) (75 mg, 0.232 mmol) 1-Hydroxybenzotriazole hydrate (31.34 mg, 0.232 mmol) and 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (66.8 mg, 0.35 mmol) in dichloromethane (3 ml) was stirred 1 h at room temperature. A solution (S)-methyl 4-(1-aminoethyl)benzoate (D3) (50 mg, 0.232 mmol) and triethylamine (0.03 ml, 0.232 mmol) in dichloromethane (1 ml) was added and the resulting mixture was stirred overnight at room temperature. NaHCO3 sat. sol. (5 ml) was added and the mixture was extracted with dichloromethane (3×10 ml). Collected organics, after solvent evaporation were purified by SPE-Si (10 g) eluting with a mixture Cyclohexane/ethylacetate from 95/05 to 60/40. Collected fractions, after solvent evaporation, afforded the title compound (D146) (100 mg).

後処理

  1. stirringthe resulting mixture was stirred overnight at room temperature
  2. extractionthe mixture was extracted with dichloromethane (3×10 ml)
  3. customCollected organics, after solvent evaporation
  4. customwere purified by SPE-Si (10 g)
  5. washeluting with a mixture Cyclohexane/ethylacetate from 95/05 to 60/40
  6. customCollected fractions, after solvent evaporation

出典と根拠

ORDレコード
ord-e8a45cd97aca4db684d6ea6e5ec381f9
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08828987B2

反応ノート

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