Lithium Chloride → (4-Amino-3-trifluoromethyl-5-vinylbenzyl)carbamic Acid tert-butyl Ester

HRID 2358389ノート

反応式

HRID 2358389 の反応式
[Li+].[Cl-].[C:3]([O:7][C:8](=[O:23])[NH:9][CH2:10][C:11]1[CH:16]=[C:15]([C:17]([F:20])([F:19])[F:18])[C:14]([NH2:21])=[C:13](I)[CH:12]=1)([CH3:6])([CH3:5])[CH3:4].[CH2:24](C([Sn])=C(CCCC)CCCC)[CH2:25]CC>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.CN(C=O)C>[C:3]([O:7][C:8](=[O:23])[NH:9][CH2:10][C:11]1[CH:12]=[C:13]([CH:24]=[CH2:25])[C:14]([NH2:21])=[C:15]([C:17]([F:20])([F:19])[F:18])[CH:16]=1)([CH3:6])([CH3:5])[CH3:4]

参加物

6

反応物 3

HCID 433294Lithium ChlorideHCID 53438229Tri(butyl)vinyltinHCID 68456058(4-Amino-3-iodo-5-trifluoromethylbenzyl)carbamic acid tert-butyl ester

生成物 1

HCID 68456886(4-Amino-3-trifluoromethyl-5-vinylbenzyl)carbamic Acid tert-butyl Ester

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 6228Dimethylformamide溶媒

実験手順

Pd(PPh3)4 (0.06 eq, 0.014 mmol, 16.64 mg) and LiCl (2.8 eq, 0.67 mmol, 28.49 mg) were added into DMF. (4-Amino-3-iodo-5-trifluoromethylbenzyl)carbamic acid tert-butyl ester (100 mg, 0.24 mmol) and tributylvinyltin (1.5 eq, 0.36 mmol, 105.37 μl) were added into the reaction mixture. The reaction mixture was stirred for 12 ha in reflux. The reaction mixture was purified according to step 4 of Example 8 to give a title product, yellow syrup (51.5 mg, 67.87%).

後処理

  1. temperaturein reflux
  2. customThe reaction mixture was purified

出典と根拠

ORDレコード
ord-1067bcd4ea6746a99d0107280fa5d252
出典データセット
uspto-grants-2010_07
特許番号
US07763657B2

反応ノート

読み込み中…