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Sodium Sulfate → ethyl (RS)-(4-cyano-phenylamino)-[3-ethyl-5-(1-methyl-piperidin-4-ylamino)-phenyl]-acetate

HRID 1066623
ノート
印刷プレビュー

反応式

HRID 1066623 の反応式
[O-]S([O-])(=O)=O.[Na+].[Na+].[NH2:8][C:9]1[CH:10]=[C:11]([CH:17]([NH:23][C:24]2[CH:29]=[CH:28][C:27]([C:30]#[N:31])=[CH:26][CH:25]=2)[C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH:12]=[C:13]([CH2:15][CH3:16])[CH:14]=1.[CH3:32][N:33]1[CH2:38][CH2:37][C:36](=O)[CH2:35][CH2:34]1.C([O-])(O)=O.[Na+]>C(O)(=O)C>[C:30]([C:27]1[CH:28]=[CH:29][C:24]([NH:23][CH:17]([C:11]2[CH:10]=[C:9]([NH:8][CH:36]3[CH2:37][CH2:38][N:33]([CH3:32])[CH2:34][CH2:35]3)[CH:14]=[C:13]([CH2:15][CH3:16])[CH:12]=2)[C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:25][CH:26]=1)#[N:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 24436Sodium SulfateHCID 740491-Methyl-4-piperidoneHCID 516892Sodium BicarbonateHCID 86583558ethyl (RS)-(3-amino-5-ethyl-phenyl)-(4-cyano-phenylamino)-acetate

生成物 1

HCID 86583561ethyl (RS)-(4-cyano-phenylamino)-[3-ethyl-5-(1-methyl-piperidin-4-ylamino)-phenyl]-acetate収率 89%

試薬・触媒・溶媒 1

HCID 176
Acetic Acid
溶媒

実験手順

Na2SO4 (1.09 g, 7.7 mmol) was added to a solution of the ethyl (RS)-(3-amino-5-ethyl-phenyl)-(4-cyano-phenylamino)-acetate (250 mg, 0.77 mmol) obtained in Example 223.4 and 1-methyl-4-piperidone (174 mg, 1.54 mmol) in acetic acid (5 ml) and the mixture was stirred for 15 min. at room temperature. The mixture was subsequently cooled to 0° C. and NaHB(OAc)3 (489 mg, 2.31 mmol) was slowly added portionwise. After 30 min. a saturated solution of NaHCO3 was added and the mixture was extracted with EtOAc. The organic phase was dried and filtered, and the filtrate was concentrated. The residue was purified by chromatography (SiO2, CH2Cl2/MeOH 9:1). There were obtained 287 mg (89%) of ethyl (RS)-(4-cyano-phenylamino)-[3-ethyl-5-(1-methyl-piperidin-4-ylamino)-phenyl]-acetate as a yellowish solid; MS: 421 ([M+H]+).

後処理

  1. temperatureThe mixture was subsequently cooled to 0° C.
  2. extractionthe mixture was extracted with EtOAc
  3. customThe organic phase was dried
  4. filtrationfiltered
  5. concentrationthe filtrate was concentrated
  6. customThe residue was purified by chromatography (SiO2, CH2Cl2/MeOH 9:1)

出典と根拠

ORDレコード
ord-239997e1792040c9a0bd3687d373f649
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06242644B1

反応ノート

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