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Indole-2-carboxylic acid → 1h-Indole-2-carboxylic acid {4-[4-(6-fluoro-benzo[b]thiophen-3-yl)-[1,4]diazepan-1-yl]-butyl}-amide

HRID 1986909
ノート
印刷プレビュー

反応式

HRID 1986909 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[C:2]1[C:10]([OH:12])=O.[F:13][C:14]1[CH:15]=[CH:16][C:17]2[C:21]([N:22]3[CH2:28][CH2:27][CH2:26][N:25]([CH2:29][CH2:30][CH2:31][CH2:32][NH2:33])[CH2:24][CH2:23]3)=[CH:20][S:19][C:18]=2[CH:34]=1.C(N(C(C)C)CC)(C)C.ON1C2C=CC=CC=2N=N1.O1CCN(N=C=N)CC1>CN(C=O)C>[F:13][C:14]1[CH:15]=[CH:16][C:17]2[C:21]([N:22]3[CH2:28][CH2:27][CH2:26][N:25]([CH2:29][CH2:30][CH2:31][CH2:32][NH:33][C:10]([C:2]4[NH:1][C:9]5[C:4]([CH:3]=4)=[CH:5][CH:6]=[CH:7][CH:8]=5)=[O:12])[CH2:24][CH2:23]3)=[CH:20][S:19][C:18]=2[CH:34]=1
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 72899Indole-2-carboxylic acidHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 20187300MorpholinocarbodiimideHCID 577225964-[4-(6-Fluoro-benzo[b]thiophen-3-yl)-[1,4]diazapan-1-yl]butylamine

生成物 1

HCID 10205110
1h-Indole-2-carboxylic acid {4-[4-(6-fluoro-benzo[b]thiophen-3-yl)-[1,4]diazepan-1-yl]-butyl}-amide
収率 53.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Add indole-2-carboxylic acid (507 mg, 3.15 mmol) to a solution of 4-[4-(6-fluoro-benzo[b]thiophen-3-yl)-[1,4]diazapan-1-yl]butylamine (Example 6) (920 mg, 2.86 mmol), diisopropylethylamine (2.5 mL, 14.3 mmol), 1-hydroxy-1H-benzotriazole (503 mg, 3.72 mmol) and morpholinocarbodiimide (1.39 g, 3.29 mmol) in DMF (10 mL), and stir the solution overnight at room temperature. Remove the solvent under vacuum and dissolve the residue in EtOAc. Wash the organic phase with ether and saturated sodium chloride solution, and dry over MgSO4. Evaporate the solvent under vacuum and purify the crude product by column chromatography (EtOAc/MeOH 7:3) to obtain 716 mg of a colorless solid LC/MS, (LiChrospher 5μ, RP-18, 250 mm CH3CN/Water-gradient 20%→100% (25 min), Flow: 1.5 mL/min) tR=19.89 min, m/z=464.3.

後処理

  1. customRemove the solvent under vacuum
  2. dissolutiondissolve the residue in EtOAc
  3. washWash the organic phase with ether and saturated sodium chloride solution
  4. dry with materialdry over MgSO4
  5. customEvaporate the solvent under vacuum
  6. custompurify the crude product by column chromatography (EtOAc/MeOH 7:3)

出典と根拠

ORDレコード
ord-af86d52deb984dd99065ffd4c150c93e
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07550469B2

反応ノート

読み込み中…

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