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Diisopropylethylamine → (1-benzenesulfonyl-5-nitro-1H-pyrrolo[2,3-b]pyridin-4-yl)-bicyclo[2.2.1]hept-2-yl-amine

HRID 1257609
ノート
印刷プレビュー

反応式

HRID 1257609 の反応式
[C:1]1([S:7]([N:10]2[C:14]3=[N:15][CH:16]=[C:17]([N+:20]([O-:22])=[O:21])[C:18](Cl)=[C:13]3[CH:12]=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:23]12[CH2:29][CH:26]([CH2:27][CH2:28]1)[CH2:25][CH:24]2[NH2:30].C(N(C(C)C)CC)(C)C>CC(O)C>[C:1]1([S:7]([N:10]2[C:14]3=[N:15][CH:16]=[C:17]([N+:20]([O-:22])=[O:21])[C:18]([NH:30][CH:24]4[CH2:25][CH:26]5[CH2:29][CH:23]4[CH2:28][CH2:27]5)=[C:13]3[CH:12]=[CH:11]2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=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

5

反応物 3

HCID 81531DiisopropylethylamineHCID 98480Exo-2-bornanamineHCID 583947741-(benzenesulfonyl)-4-chloro-5-nitro-1H-pyrrolo(2,3-b)pyridine

生成物 1

HCID 67343346(1-benzenesulfonyl-5-nitro-1H-pyrrolo[2,3-b]pyridin-4-yl)-bicyclo[2.2.1]hept-2-yl-amine収率 98.8%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
110 °C

実験手順

A mixture of 1-benzenesulfonyl-4-chloro-5-nitro-1H-pyrrolo[2,3-b]pyridine (0.92 g, 2.7 mmol), bicyclo[2.2.1]hept-2-ylamine (0.36 ml, 3.0 mmol), diisopropylethylamine (0.62 ml, 3.5 mmol) in propan-2-ol (12 ml) was heated at 110° C. in a microwave reactor for 20 min. The mixture was then cooled to 25° C. and was partitioned between water (200 ml) and EtOAc (2×200 ml). The combined organic layers were dried over MgSO4, filtered, and the filtrate was concentrated under reduced pressure. Purification of the resulting yellow oil by column chromatography on silica gel (gradient: 0 to 60% EtOAc in heptanes) afforded (1-benzenesulfonyl-5-nitro-1H-pyrrolo[2,3-b]pyridin-4-yl)-bicyclo[2.2.1]hept-2-yl-amine (1.1 g, 98%) as a yellow solid. TLC: 50% EtOAc in heptanes; Rf=0.66). This material was used in the next step below without additional characterization.

後処理

  1. temperatureThe mixture was then cooled to 25° C.
  2. customwas partitioned between water (200 ml) and EtOAc (2×200 ml)
  3. dry with materialThe combined organic layers were dried over MgSO4
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customPurification of the resulting yellow oil by column chromatography on silica gel (gradient: 0 to 60% EtOAc in heptanes)

出典と根拠

ORDレコード
ord-f114f67c1a5c457aa097eb15c14998d8
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461328B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート