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Sodium Carbonate → HCID 66549142、化合物

HRID 1410054
ノート
印刷プレビュー

反応式

HRID 1410054 の反応式
Cl[C:2]1[N:3]=[C:4]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[C:14]([O:20][CH3:21])[CH:13]=2)[C:5]2[N:10]=[CH:9][S:8][C:6]=2[N:7]=1.CC1(C)C(C)(C)OB([C:30]2[CH:31]=[C:32]([CH:48]=[CH:49][CH:50]=2)[CH2:33][NH:34][C:35]2[CH:47]=[CH:46][C:38]([C:39]([O:41][C:42]([CH3:45])([CH3:44])[CH3:43])=[O:40])=[CH:37][CH:36]=2)O1.C([O-])([O-])=O.[Na+].[Na+]>O.O1CCOCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH3:21][O:20][C:14]1[CH:13]=[C:12]([NH:11][C:4]2[C:5]3[N:10]=[CH:9][S:8][C:6]=3[N:7]=[C:2]([C:30]3[CH:31]=[C:32]([CH:48]=[CH:49][CH:50]=3)[CH2:33][NH:34][C:35]3[CH:47]=[CH:46][C:38]([C:39]([O:41][C:42]([CH3:45])([CH3:43])[CH3:44])=[O:40])=[CH:37][CH:36]=3)[N:3]=2)[CH:17]=[CH:16][C:15]=1[O:18][CH3:19]
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 3

HCID 10340Sodium CarbonateHCID 68379697HCID 68379697、化合物HCID 715341855-chloro-N-(3,4-dimethoxyphenyl)thiazolo[5,4-d]pyrimidin-7-amine

生成物 1

HCID 66549142HCID 66549142、化合物収率 41%

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒
HCID 962
Water
溶媒
HCID 312751,4-Dioxane溶媒

実験手順

Under N2 atmosphere, 5-chloro-N-(3,4-dimethoxyphenyl)thiazolo[5,4-d]pyrimidin-7-amine (100 mg, 0.31 mmol), tert-butyl 4-(3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzylamino)benzoate (150 mg, crude), Pd(PPh3)4 (30 mg, 0.026 mmol) and Na2CO3 (150 mg, 1.41 mmol) in 5 mL of water was added in 30 mL of 1,4-dioxane. The mixture was stirred at reflux for 18 hours. The solvent was removed under reduce pressure and the residue was purified by silica gel chromatography, eluting with petroleum ether and ethyl acetate (5:1) to give tert-butyl 4-(3-(7-(3,4-dimethoxyphenylamino)thiazolo[5,4-d]pyrimidin-5-yl)benzylamino)benzoate (72 mg, 41%) as a yellow sold. 1H NMR (300 MHz, DMSO): δ 8.87 (s, 1H), 8.54-8.47 (m, 2H), 7.86-7.82 (m, 3H), 7.49-7.28 (m, 2H), 7.27-7.23 (m, 1H), 6.94 (d, 1H, J=8.7 Hz), 6.65-6.62 (m, 2H), 4.49 (s, 2H), 4.16 (s, 3H), 4.13 (s, 3H). LC-MS: 570 [M+H]+, tR=1.83 min. HPLC: 98.31% at 214 nm, 98.91% at 254 nm, tR=8.06 min.

後処理

  1. temperatureat reflux for 18 hours
  2. customThe solvent was removed
  3. customthe residue was purified by silica gel chromatography
  4. washeluting with petroleum ether and ethyl acetate (5:1)

出典と根拠

ORDレコード
ord-36989776d681434a9df9ae835dbe4982
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08921383B2

反応ノート

読み込み中…

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