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1,2-Dichloroethane → HCID 58646024、化合物

HRID 1171895
ノート
印刷プレビュー

反応式

HRID 1171895 の反応式
[NH2:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][CH2:7][N:8]2[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])=[CH:4][CH:3]=1.CCN(C(C)C)C(C)C.Cl.[N:28]1[C:37]2[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=2)[C:31]([CH2:38][NH:39][C:40]2[CH:44]=[CH:43][S:42][C:41]=2[C:45](O)=[O:46])=[CH:30][CH:29]=1.C(Cl)CCl.C1C=NC2N(O)N=NC=2C=1>C(Cl)Cl.CN(C1C=CN=CC=1)C>[N:28]1[C:37]2[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=2)[C:31]([CH2:38][NH:39][C:40]2[CH:44]=[CH:43][S:42][C:41]=2[C:45]([NH:1][C:2]2[CH:10]=[C:9]3[C:5]([CH2:6][CH2:7][N:8]3[C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])=[CH:4][CH:3]=2)=[O:46])=[CH:30][CH:29]=1
参加物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 111,2-DichloroethaneHCID 81531DiisopropylethylamineHCID 181649HOAtHCID 21936857tert-Butyl 6-amino-2,3-dihydro-1H-indole-1-carboxylateHCID 68767362HCID 68767362、化合物

生成物 1

HCID 58646024HCID 58646024、化合物

試薬・触媒・溶媒 2

HCID 14284
4-(Dimethylamino)pyridine
触媒
HCID 6344Dichloromethane溶媒

実験手順

To a solution of tert-butyl 6-aminoindoline-1-carboxylate (3.2 g, 13.68 mmol) in CH2Cl2 (135 mL) was added iPr2NEt (14 mL), 3-[(quinolin-4-ylmethyl)amino]thiophene-2-carboxylic acid hydrochloride (5.27 g, 16.42 mmol), EDC (3.93 g, 20.5 mmol), DMAP (0.81 g, 6.63 mmol), and HOAt (5.5 mL. 0.5M in DMF). The resulting mixture was then heated to reflux under N2 atmosphere. After 8 h the reaction was cooled to rt and then washed with 50% NaCl solution. The organic layer was dried over Na2SO4, filtered, and concentrated in vacuo to yield a residue that was purified by silica gel chromatography (80% EtOAc in Hexanes 100% EtOAc) to yield tert-butyl 6-({[3-[(quinolin-4-ylmethyl)amino]thien-2-yl]carbonyl}amino)indoline-1-carboxylate as a yellow solid. MS (ES+): m/z 501 [M+1]. 1H NMR (d6-DMSO, 400 MHz): δ1.48 (s, 9H), 2.99 (t, J=8.4 Hz, 2H), 3.90 (t, J=8.4 Hz, 2H), 5.06 (d, J=6.0 Hz, 2H), 6.78 (brs, 1H), 7.07 (d, J=8.4 Hz, 1H), 7.40 (d, J=4.4 Hz, 1H), 7.56 (d, J=5.6 Hz, 1H), 7.66 (t, J=6.8 Hz, 1H), 7.78 (t, J=6.8 Hz, 1H), 8.04 (m, 2H), 8.21 (d, J=8.0 Hz, 1H), 8.82 (d, J=4.4 Hz, 1H), 9.35 (s, 1H).

後処理

  1. temperatureThe resulting mixture was then heated
  2. temperatureto reflux under N2 atmosphere
  3. washwashed with 50% NaCl solution
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customto yield a residue that
  8. customwas purified by silica gel chromatography (80% EtOAc in Hexanes 100% EtOAc)

出典と根拠

ORDレコード
ord-e1066bb4f6d947c39a0faa53480797d0
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07829717B2

反応ノート

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