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Triethylamine → 6-Amino-1H-pyrrolo[2,3-b]pyridine-5-carboxylic acid (5-phenoxy-thiophen-2-ylmethyl)-amide

HRID 2080256
ノート
印刷プレビュー

反応式

HRID 2080256 の反応式
C(O[C:4]([C:6]1[CH:7]=[C:8]2[CH:15]=[CH:14][NH:13][C:9]2=[N:10][C:11]=1[NH2:12])=[O:5])C.[OH-].[Na+].C(N(CC)CC)C.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)C2C=CC=CC=2N=N1.[O:52]([C:59]1[S:63][C:62]([CH2:64][NH2:65])=[CH:61][CH:60]=1)[C:53]1[CH:58]=[CH:57][CH:56]=[CH:55][CH:54]=1>C(O)C.[Cl-].[Na+].O>[O:52]([C:59]1[S:63][C:62]([CH2:64][NH:65][C:4]([C:6]2[CH:7]=[C:8]3[CH:15]=[CH:14][NH:13][C:9]3=[N:10][C:11]=2[NH2:12])=[O:5])=[CH:61][CH:60]=1)[C:53]1[CH:54]=[CH:55][CH:56]=[CH:57][CH:58]=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 8471TriethylamineHCID 14798Sodium HydroxideHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 23130515C-(5-Phenoxy thiophen-2-yl)methylamineHCID 58387889Ethyl 6-amino-1H-pyrrolo[2,3-B]pyridine-5-carboxylate

生成物 1

HCID 58388004
6-Amino-1H-pyrrolo[2,3-b]pyridine-5-carboxylic acid (5-phenoxy-thiophen-2-ylmethyl)-amide
収率 18.5%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 57417360Sodium chloride; water溶媒

反応条件

温度
98 °C

実験手順

To a solution of 6-amino-1H-pyrrolo[2,3-b]pyridine-5-carboxylic acid ethyl ester described in Preparation Example R-2 (95 mg, 0.46 mmol) in ethanol (10 mL) was added an aqueous solution of 1N sodium hydroxide (5 mL, 5 mmol), which was then heated for 3 hours in an oil bath at 98° C. After cooling the reaction solution, the reaction solution was concentrated until it reached ⅓ of its volume, neutralized with 1N hydrochloric acid, and further concentrated. The resulting crude product was suspended in N,N-dimethylformamide (5 mL), triethylamine (0.096 mL, 0.69 mmol), benzotriazol-1-yloxytris(dimethylamino)phosphonium hexafluorophosphate (153 mg, 0.35 mmol) and C-(5-phenoxy-thiophen-2-yl)-methylamine described in Preparation Example 26 (71 mg, 0.35 mmol) were added thereto, followed by stirring at room temperature for 15 hours. After the reaction was completed, the reaction solution was poured into brine, and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, then concentrated, the obtained residue was purified by silica gel column chromatography (ethyl acetate:hexane=2:1), and the title compound (31 mg, 0.085 mmol, 18.5%) was obtained.

後処理

  1. temperatureAfter cooling the reaction solution
  2. concentrationthe reaction solution was concentrated until it
  3. concentrationfurther concentrated
  4. additionwere added
  5. extractionextracted with ethyl acetate
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated
  8. customthe obtained residue was purified by silica gel column chromatography (ethyl acetate:hexane=2:1)

出典と根拠

ORDレコード
ord-d38dbe60c48d472faf6e09d792b6defc
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07932272B2

反応ノート

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