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Hydrochloric Acid → 21-Chloro-10-oxa-2,19,23,24-tetrazatetracyclo[18.3.1.13,7.111,15]hexacosa-1(23),3,5,7(26),11,13,15(25),20(24),21-nonaene

HRID 1614966
ノート
印刷プレビュー

反応式

HRID 1614966 の反応式
Br[CH2:2][CH2:3][C:4]1[CH:5]=[C:6]([NH:10][C:11]2[N:16]=[C:15]([NH:17][CH2:18][CH2:19][CH2:20][C:21]3[CH:22]=[C:23]([OH:27])[CH:24]=[CH:25][CH:26]=3)[C:14]([Cl:28])=[CH:13][N:12]=2)[CH:7]=[CH:8][CH:9]=1.[OH-].[Na+].Cl>O1CCCC1.O>[Cl:28][C:14]1[CH:13]=[N:12][C:11]2=[N:16][C:15]=1[NH:17][CH2:18][CH2:19][CH2:20][C:21]1[CH:22]=[C:23]([O:27][CH2:2][CH2:3][C:4]3[CH:5]=[C:6]([NH:10]2)[CH:7]=[CH:8][CH:9]=3)[CH:24]=[CH:25][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 58467888HCID 58467888、化合物

生成物 1

HCID 4686474621-Chloro-10-oxa-2,19,23,24-tetrazatetracyclo[18.3.1.13,7.111,15]hexacosa-1(23),3,5,7(26),11,13,15(25),20(24),21-nonaene収率 11%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒

実験手順

To a solution of 3-{3-[(2-{[3-(2-bromoethyl)phenyl]amino}-5-chloropyrimidin-4-yl)amino]propyl}phenol (50.0 mg, 0.108 mmol) in tetrahydrofuran (1.0 mL) was added a solution of sodium hydroxide in water (1.0 mL, 1.0 M). The resultant solution was stirred at rt for 60 hours until the reaction was complete. The reaction mixture was neutralized with HCl (3 M aqueous solution) to pH=7. The aqueous layer was extracted with EtOAc three times. The combined organic layers were dried over Na2SO4, filtered, and concentrated to give the crude, which was purified by silica gel column chromatography to give the desired product as a white powder (4.5 mg, 11%). LCMS for C21H22ClN4O (M+H)+: m/z=381.0. 1H NMR (400 MHz, CD3OD): δ 7.98 (s, 1H), 7.92 (s, 1H), 7.48 (d, J=7.6 Hz, 1H), 7.40 (m, 1H), 7.06 (m, 1H), 6.97 (s, 1H), 6.70 (d, J=2.4 Hz, 1H), 6.62 (m, 2H), 3.60 (m, 4H), 3.20 (m, 2H), 2.68 (t, J=7.6 Hz, 2H), 2.02 (t, J=7.6 Hz, 2H).

後処理

  1. extractionThe aqueous layer was extracted with EtOAc three times
  2. dry with materialThe combined organic layers were dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto give the crude, which
  6. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-fed1cec749944667b9b441390aa4c4a5
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765727B2

反応ノート

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