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

HRID 2358389노트

반응식

HRID 2358389 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 6228Dimethylformamide용매

실험 절차

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%).

후처리

  1. temperaturein reflux
  2. customThe reaction mixture was purified

출처 및 근거

ORD 기록
ord-1067bcd4ea6746a99d0107280fa5d252
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07763657B2

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