4-Toluenesulfonyl chloride → HCID 53810576, 화합물

HRID 2287041노트

반응식

HRID 2287041 반응식
[NH2:1][CH:2]([CH2:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=1)[C:3]([CH3:9])([CH3:8])[C:4]([O:6][CH3:7])=[O:5].C(N(CC)CC)C.[C:26]1([CH3:36])[CH:31]=[CH:30][C:29]([S:32](Cl)(=[O:34])=[O:33])=[CH:28][CH:27]=1>C(Cl)(Cl)Cl>[CH3:9][C:3]([CH3:8])([CH:2]([NH:1][S:32]([C:29]1[CH:30]=[CH:31][C:26]([CH3:36])=[CH:27][CH:28]=1)(=[O:34])=[O:33])[CH2:10][C:11]1[CH:12]=[CH:13][C:14]([O:17][CH3:18])=[CH:15][CH:16]=1)[C:4]([O:6][CH3:7])=[O:5]

참가 물질

5

반응물 3

HCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 23460866HCID 23460866, 화합물

생성물 1

HCID 53810576HCID 53810576, 화합물수율 85%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

To a solution of 251 g of methyl 3-amino-2,2-dimethyl-4-(p-methoxyphenyl)butyrate and 121 g of triethylamine in 750 ml of chloroform, there is added, with mechanical stirring and cooling with ice water, a solution of 210 g of p-toluenesulphonyl chloride in 500 ml of chloroform. After completion of the addition, which is carried out at such a rate that the temperature of the reaction mixture does not exceed 25° C., stirring is continued for 1.5 hours. Then the solution is washed with water, dilute hydrochloric acid and again with water, subsequently. After drying, the organic solvent is stripped off in vacuo. The residue is treated with ether, resulting in the crystallization of the title compound.

후처리

  1. additionAfter completion of the addition, which
  2. customdoes not exceed 25° C.
  3. stirringstirring
  4. washThen the solution is washed with water, dilute hydrochloric acid and again with water
  5. customAfter drying
  6. additionThe residue is treated with ether

출처 및 근거

ORD 기록
ord-afbf2d98918f4590bda6abec77df1668
출처 데이터셋
uspto-grants-1981_05
특허 번호
US04268673

반응 노트

불러오는 중…