1,2-Dichloroethane → Ethyl 1-({[(tert-butoxycarbonyl)amino][3-(trifluoromethyl)phenyl]acetyl}amino)cyclopropanecarboxylate

HRID 574147

反応式

HRID 574147 の反応式
[C:1]([O:5][C:6]([NH:8][CH:9]([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:22])([F:21])[F:20])[CH:14]=1)[C:10](O)=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:23][C:24]1([C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH2:26][CH2:25]1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C.C(OCC)(=O)C>[C:1]([O:5][C:6]([NH:8][CH:9]([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([F:20])([F:21])[F:22])[CH:14]=1)[C:10]([NH:23][C:24]1([C:27]([O:29][CH2:30][CH3:31])=[O:28])[CH2:26][CH2:25]1)=[O:11])=[O:7])([CH3:2])([CH3:3])[CH3:4]

参加物

7

反応物 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 386204Ethyl 1-aminocyclopropanecarboxylateHCID 223091762-{[(Tert-butoxy)carbonyl]amino}-2-[3-(trifluoromethyl)phenyl]acetic acid

生成物 1

HCID 66801809Ethyl 1-({[(tert-butoxycarbonyl)amino][3-(trifluoromethyl)phenyl]acetyl}amino)cyclopropanecarboxylate

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 500 mg (1.57 mmol) of [(tert-butoxycarbonyl)amino][3-(trifluoromethyl)-phenyl]acetic acid, 243 mg (1.88 mmol) of ethyl 1-aminocyclopropanecarboxylate, 450 mg (2.35 mmol) of EDC and 317 mg (2.35 mmol) of HOBt in 10 ml of DMF was stirred at RT overnight. The reaction mixture was diluted with ethyl acetate and washed twice with 1N hydrochloric acid and once with a saturated aqueous sodium bicarbonate solution. The organic phase was dried over sodium sulphate and then freed from the solvent on a rotary evaporator. The residue was dried under high vacuum. This gave 650 mg (96% of theory) of the title compound.

後処理

  1. washwashed twice with 1N hydrochloric acid and once with a saturated aqueous sodium bicarbonate solution
  2. dry with materialThe organic phase was dried over sodium sulphate
  3. customfreed from the solvent on a rotary evaporator
  4. customThe residue was dried under high vacuum

出典と根拠

ORDレコード
ord-bdcae72e96dc4e69890096b6d291c9c9
出典データセット
uspto-grants-2015_05
特許番号
US09034855B2

関連ノート

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