3-Chloroaniline → HCID 18663372, 화합물

HRID 1956686노트

반응식

HRID 1956686 반응식
[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]#[C:22][CH3:23])[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][C:21]#[C:22][CH3:23])[CH2:18][NH:5][C:4]1[CH:6]=[CH:7][CH:8]=[C:2]([Cl:1])[CH:3]=1)=[O:15])([CH3:12])([CH3:11])[CH3:10]

참가 물질

6

반응물 4

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

생성물 1

HCID 18663372HCID 18663372, 화합물

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

To a 0° C. solution of 3-chloroaniline (4.33 mL, 40.9 mmol), the product from Step K (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.

후처리

  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

출처 및 근거

ORD 기록
ord-1091ce6b8c374d6cb8f3f4569d03fb08
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05780492

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