Trifluoroacetic acid → HCID 21097464、化合物

HRID 1350820

反応式

HRID 1350820 の反応式
[C:1]([C:5]1[CH:19]=[CH:18][C:8]([O:9][CH2:10][C:11]([O:13]C(C)(C)C)=O)=[CH:7][C:6]=1[O:20][CH3:21])([CH3:4])([CH3:3])[CH3:2].FC(F)(F)C(O)=O.C(C1C=CC(OCC(O)=O)=CC=1OC)(C)(C)C.[Cl-].ClC1N(C)CC[NH+]1C.Cl.[NH2:56][CH2:57][C:58]1[CH:63]=[CH:62][C:61]([NH:64][S:65]([CH3:68])(=[O:67])=[O:66])=[C:60]([F:69])[CH:59]=1>C(N(CC)CC)C.C(Cl)Cl.O1CCCC1>[C:1]([C:5]1[CH:19]=[CH:18][C:8]([O:9][CH2:10][C:11]([NH:56][CH2:57][C:58]2[CH:63]=[CH:62][C:61]([NH:64][S:65]([CH3:68])(=[O:67])=[O:66])=[C:60]([F:69])[CH:59]=2)=[O:13])=[CH:7][C:6]=1[O:20][CH3:21])([CH3:2])([CH3:3])[CH3:4]

参加物

9

反応物 5

HCID 6422Trifluoroacetic acidHCID 109867151H-Imidazolium, 2-chloro-4,5-dihydro-1,3-dimethyl-, chlorideHCID 21097506HCID 21097506、化合物HCID 21097525HCID 21097525、化合物HCID 58640411tert-Butyl (4-tert-butyl-3-methoxyphenoxy)acetate

生成物 1

HCID 21097464HCID 21097464、化合物収率 2.9%

試薬・触媒・溶媒 3

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒

実験手順

A mixture of tert butyl (4-tert-butyl-3-methoxyphenoxy)acetate (466 mg, 1.6 mmol), trifluoroacetic acid (2.0 ml), tetrahydrofuran (THF) (3.0 ml) and methylene dichloride (2.0 ml) was stirred for 1 hour at ambient temperature. After being concentrated under reduced pressure, the residue was used for further reaction without purification (460 mg). Then (4-tert-butyl-3-methoxyphenoxy)acetic acid (460 mg, crude), 2-chloro-1,3-dimethylimidazolinium chloride (CDI) (97 mg, 0.6 mmol), triethylamine (0.33 ml) and N-[4-(aminomethyl)-2-fluorophenyl]methanesulfonamide hydrochloride (160 mg, 0.63 mmol) were treated in the same procedure described in Example 2(b) to give 8.1 mg (1.1% yield) of the title compound as a white solid.

後処理

  1. concentrationAfter being concentrated under reduced pressure
  2. customthe residue was used for further reaction without purification (460 mg)

出典と根拠

ORDレコード
ord-e01ed5d8b61849ef943c96dd93bdc247
出典データセット
uspto-grants-2007_05
特許番号
US07214824B2

関連ノート

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