Piperidine → HCID 178510302、化合物

HRID 527272

反応式

HRID 527272 の反応式
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[CH:9]=2)[C:3]=1[C:15]#[N:16].[OH:17][CH2:18][CH2:19][O:20][C:21]1[CH:28]=[CH:27][C:24]([CH:25]=O)=[CH:23][CH:22]=1.N1CCCCC1.[BH4-].[Na+]>C(O)C.CO>[Cl:14][C:10]1[CH:9]=[C:8]([NH:7][C:4]2[C:3]([C:15]#[N:16])=[C:2]([NH:1][CH2:25][C:24]3[CH:23]=[CH:22][C:21]([O:20][CH2:19][CH2:18][OH:17])=[CH:28][CH:27]=3)[NH:6][N:5]=2)[CH:13]=[CH:12][CH:11]=1

参加物

7

反応物 4

HCID 8082PiperidineHCID 89178Benzaldehyde, 4-(2-hydroxyethoxy)-HCID 4311764Sodium borohydrideHCID 106811675-Amino-3-(3-chloro-phenylamino)-4-cyano-pyrazole

生成物 1

HCID 178510302HCID 178510302、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 887Methanol溶媒

反応条件

温度
85 °C

実験手順

Dissolved 5-amino-3-((3-chlorophenyl)amino)-1H-pyrazole-4-carbonitrile (58 mg) in 4 mL ethanol and added 0.250 mmol of 4(2-hydroxyethoxy)benzaldehyde followed by a single drop of piperidine. This solution was then heated to 85° C. for 17 hrs, then the ethanol was evaporated and the resulting product was scraped from the reaction vessels. The powder was then resuspended in 4 mL of MeOH and 3 eq. of sodium borohydride was added and left stirring overnight at room temperature. Then MeOH was then evaporated and the product C21 was scraped and collected. (100 mg)

後処理

  1. customthe ethanol was evaporated
  2. customthe resulting product was scraped from the reaction vessels
  3. waitleft
  4. customThen MeOH was then evaporated
  5. customcollected

出典と根拠

ORDレコード
ord-14bec02312b64e56861a311d268b324f
出典データセット
uspto-grants-2016_05
特許番号
US09346792B2

関連ノート

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