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1-Hydroxybenzotriazole → HCID 24965744、化合物

HRID 420128
ノート
印刷プレビュー

反応式

HRID 420128 の反応式
[C:1]([C:4]1[C:12]2[C:7](=[CH:8][C:9]([C:16](O)=[O:17])=[CH:10][C:11]=2[O:13][CH2:14][CH3:15])[N:6]([CH:19]2[CH2:21][CH2:20]2)[CH:5]=1)(=[O:3])[NH2:2].Cl.[CH3:23][O:24][C:25](=[O:48])[C:26]1[CH:31]=[CH:30][CH:29]=[C:28]([C:32]2[CH:33]=[C:34]3[C:44](=[CH:45][CH:46]=2)[O:43][C:37]2([CH2:42][CH2:41][NH:40][CH2:39][CH2:38]2)[CH2:36][C:35]3=[O:47])[CH:27]=1.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C.C(OCC)(=O)C.C(N(CC)CC)C>[C:1]([C:4]1[C:12]2[C:7](=[CH:8][C:9]([C:16]([N:40]3[CH2:39][CH2:38][C:37]4([CH2:36][C:35](=[O:47])[C:34]5[C:44](=[CH:45][CH:46]=[C:32]([C:28]6[CH:27]=[C:26]([CH:31]=[CH:30][CH:29]=6)[C:25]([O:24][CH3:23])=[O:48])[CH:33]=5)[O:43]4)[CH2:42][CH2:41]3)=[O:17])=[CH:10][C:11]=2[O:13][CH2:14][CH3:15])[N:6]([CH:19]2[CH2:21][CH2:20]2)[CH:5]=1)(=[O:3])[NH2:2]
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 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 66649548HCID 66649548、化合物HCID 66649562HCID 66649562、化合物

生成物 1

HCID 24965744HCID 24965744、化合物

試薬・触媒・溶媒 3

HCID 6228
Dimethylformamide
溶媒
HCID 8471Triethylamine溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

Triethylamine (0.22 mL) was added to a solution of 3-carbamoyl-1-cyclopropyl-4-ethoxy-1H-indole-6-carboxylic acid (229 mg), 3-(4-oxo-spiro[chroman-2,4′-piperidin]-6-yl)benzoic acid methyl ester hydrochloride (306 mg), WSC hydrochloride (166 mg) and HOBT (133 mg) in DMF (4 mL), and the mixture was stirred at 60° C. for 1 hour. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate, then washed successively with water, aqueous saturated sodium bicarbonate and saturated saline water. The organic layer was dried over sodium sulfate, filtered, concentrated, and purified through silica gel column chromatography (chloroform/methanol) to obtain the intended ester derivative as a colorless amorphous substance. 1H-NMR (400 MHz, CDCl3) δ: 8.71 (1H, s), 8.25 (1H, dd, J=1.5, 1.5 Hz), 8.14 (1H, d, J=2.4 Hz), 8.04-8.00 (2H, m), 7.83-7.74 (2H, m), 7.51 (1H, dd, J=7.8, 7.8 Hz), 7.37 (1H, d, J=1.5 Hz), 7.13 (1H, d, J=7.8 Hz), 6.74 (1H, d, J=1.5 Hz), 5.54 (1H, s), 4.62-4.41 (1H, br m), 4.29 (2H, q, J=7.0 Hz), 3.95 (3H, s), 2.28-1.71 (4H, br m), 3.88-3.32 (4H, br m), 2.82 (2H, s), 1.55 (3H, t, J=7.0 Hz), 1.16-1.00 (4H, m); MS [M+H]+=622.

後処理

  1. temperatureAfter cooling to room temperature
  2. washwashed successively with water, aqueous saturated sodium bicarbonate and saturated saline water
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. custompurified through silica gel column chromatography (chloroform/methanol)

出典と根拠

ORDレコード
ord-a07f7ad9c8d549d69cee97eeba63d14c
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08093389B2

反応ノート

読み込み中…

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