3-Chloroaniline → HCID 54469342、化合物

HRID 342147ノート

反応式

HRID 342147 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].[C:9]([O:13][C:14]([NH:16][CH:17]([CH2:20][C:21]#CC)[CH:18]=O)=[O:15])([CH3:12])([CH3:11])[CH3:10].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].CCOC(C)=O>ClC(Cl)C>[C:9]([O:13][C:14]([NH:16][CH:17]([CH2:20][CH2:21][NH:5][C:4]1[CH:6]=[CH:7][CH:8]=[C:2]([Cl:1])[CH:3]=1)[CH3:18])=[O:15])([CH3:12])([CH3:11])[CH3:10]

参加物

6

反応物 4

HCID 79323-ChloroanilineHCID 8857Ethyl AcetateHCID 5049666Sodium triacetoxyborohydrideHCID 45092115Tert-butyl N-(1-oxohex-4-YN-2-YL)carbamate

生成物 1

HCID 54469342HCID 54469342、化合物

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

To a 0° C. solution of 3-chloroaniline (4.33 mL, 40.9 mmol), the product from Step F (ca. 41 mmol), and crushed 4 Å molecular sieves (10 g) in dichloroethane (100 mL) under nitrogen was added sodium triacetoxyborohydride (12.9 g, 61.5 mmol). The reaction was stirred for one hour, then warmed to room temperature. After 3 hours, the solution was poured into EtOAc and washed with water, sat. NaHCO3 soln. and brine. The solution was dried over sodium sulfate and concentrated in vacuo to provide the crude product.

後処理

  1. waitAfter 3 hours
  2. washwashed with water, sat. NaHCO3 soln
  3. dry with materialThe solution was dried over sodium sulfate
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-37775437f4784060b1ac8190658d5783
出典データセット
uspto-grants-1999_01
特許番号
US05856326

反応ノート

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