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Ethanol → HCID 145857641、化合物

HRID 723248
ノート
印刷プレビュー

反応式

HRID 723248 の反応式
[CH3:1][Si:2]([CH3:27])([CH3:26])[CH2:3][CH2:4][O:5][C:6](=[O:25])[NH:7][C:8]1[CH:13]=[C:12]([CH3:14])[C:11](B2OC(C)(C)C(C)(C)O2)=[C:10]([NH2:24])[CH:9]=1.[C:28]([O:32][C:33](=[O:54])[NH:34][C:35]([C:37]1[S:38][C:39]([S:52][CH3:53])=[C:40]([S:42]([C:45]2[CH:50]=[CH:49][CH:48]=[C:47](Br)[CH:46]=2)(=[O:44])=[O:43])[CH:41]=1)=[NH:36])([CH3:31])([CH3:30])[CH3:29].C([O-])([O-])=O.[Na+].[Na+].C(O)C>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.O.CCOC(C)=O.C1(C)C=CC=CC=1>[CH3:27][Si:2]([CH3:1])([CH3:26])[CH2:3][CH2:4][O:5][C:6](=[O:25])[NH:7][C:8]1[CH:9]=[C:10]([NH2:24])[C:11]([C:49]2[CH:48]=[CH:47][CH:46]=[C:45]([S:42]([C:40]3[CH:41]=[C:37]([C:35]([NH:34][C:33]([O:32][C:28]([CH3:29])([CH3:30])[CH3:31])=[O:54])=[NH:36])[S:38][C:39]=3[S:52][CH3:53])(=[O:43])=[O:44])[CH:50]=2)=[C:12]([CH3:14])[CH:13]=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

9

反応物 4

HCID 702EthanolHCID 10340Sodium CarbonateHCID 57532218HCID 57532218、化合物HCID 145857672tert-butyl N-[4-(3-bromophenyl)sulfonyl-5-methylsulfanylthiophene-2-carboximidoyl]carbamate

生成物 1

HCID 145857641HCID 145857641、化合物収率 55.5%

試薬・触媒・溶媒 4

HCID 178418397
HCID 178418397、化合物
触媒
HCID 962Water溶媒
HCID 1140Toluene溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

A flask with a stirbar was charged with [3-amino-5-methyl-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenyl]-carbamic acid 2-trimethylsilanyl-ethyl ester ((Example 294: step e) 2.34 g, 5.96 mmol), {[4-(3-bromo-benzenesulfonyl)-5-methylsulfanyl-thiophen-2-yl]-imino-methyl}-carbamic acid tert-butyl ester ((Example 27: step c) 2.93 g, 5.96 mmol), aqueous Na2CO3 (2M, 11.9 mL, 23.8 mmol), ethanol (12 mL) and toluene (24 mL). The solution was sparged with argon for 10 min and Pd(PPh3)4 (689 mg, 0.6 mmol) was added. The biphasic solution was vigorously stirred under inert atmosphere at 80° C. for 16 h, then was cooled to rt. EtOAc (80 mL) and water (20 mL) were added and the layers were separated. The organic layer was washed with saturated NaHCO3 (2×20 mL), brine (20 mL) and was dried over sodium sulfate. Removal of the solvents in vacuo followed by column chromatography (85:15 DCM/EtOAc) of the residue yielded the title compound (2.24 g, 55%) as a light brown solid. 1H-NMR (CDCl3): δ 7.98 (ddd, 1H, J=1.3, 1.9, 7.8 Hz), 7.89 (m, 2H), 7.61 (t, 1H, J=7.7 Hz), 7.5 (dt, 1H, J=1.3, 7.7 Hz), 6.88 (s, 1H), 6.55 (d, 1H, J=1.7 Hz), 6.47 (s, 1H), 4.26 (m, 2H), 3.42 (s, 2H), 2.56 (s, 3H), 1.9 (s, 3H), 1.52 (s, 9H), 1.06 (m, 2H), 0.08 (s, 9H).

後処理

  1. customThe solution was sparged with argon for 10 min
  2. temperaturewas cooled to rt
  3. customthe layers were separated
  4. washThe organic layer was washed with saturated NaHCO3 (2×20 mL), brine (20 mL)
  5. dry with materialwas dried over sodium sulfate
  6. customRemoval of the solvents in vacuo

出典と根拠

ORDレコード
ord-4a9d60dbdaeb44ceb1ab4622b68bf1d8
出典データセット
uspto-grants-2006_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07138530B2

反応ノート

読み込み中…

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