Water → Phenyl(6-thiocyanato-1,3-benzothiazol-2-yl)carbamate

HRID 1035753

반응식

HRID 1035753 반응식
[C:1](Cl)(=[O:9])[O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(=O)([O-])O.[Na+].O.[NH2:17][C:18]1[S:19][C:20]2[CH:26]=[C:25]([S:27][C:28]#[N:29])[CH:24]=[CH:23][C:21]=2[N:22]=1>O1CCCC1>[S:27]([C:25]1[CH:24]=[CH:23][C:21]2[N:22]=[C:18]([NH:17][C:1](=[O:9])[O:2][C:3]3[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=3)[S:19][C:20]=2[CH:26]=1)[C:28]#[N:29]

참가 물질

6

반응물 4

HCID 962WaterHCID 15891Phenyl chloroformateHCID 816002-Amino-6-thiocyanato-1,3-benzothiazoleHCID 516892Sodium Bicarbonate

생성물 1

HCID 53472570Phenyl(6-thiocyanato-1,3-benzothiazol-2-yl)carbamate수율 87.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
20 °C

실험 절차

7.5 g of phenyl chlorocarbonate and then 4.05 g of sodium hydrogen carbonate and 9.4 cm3 of water are added, at 20° C., to a solution of 2.5 g of commercial 2-amino-1,3-benzothiazol-6-yl thiocyanate in 94 cm3 of tetrahydrofuran. The resulting mixture is subsequently stirred at 20° C. for 20 h and then extracted with 2×150 cm3 of ethyl acetate. The organic phases are combined and then washed with 3×50 cm3 of a saturated aqueous solution of sodium hydrogen carbonate. The organic phase obtained is dried over magnesium sulphate and then concentrated to dryness under reduced pressure. The residue is taken up in 50 cm3 of water and the product is spin-filter-dried and dried under vacuum at 20° C. 3.45 g of phenyl (6-thiocyanato-1,3-benzothiazol-2-yl)carbamate are thus obtained in the form of a pale yellow solid, the characteristics of which are as follows:

후처리

  1. extractionextracted with 2×150 cm3 of ethyl acetate
  2. washwashed with 3×50 cm3 of a saturated aqueous solution of sodium hydrogen carbonate
  3. customThe organic phase obtained
  4. dry with materialis dried over magnesium sulphate
  5. concentrationconcentrated to dryness under reduced pressure
  6. customthe product is spin-filter-dried
  7. customdried under vacuum at 20° C

출처 및 근거

ORD 기록
ord-c93db23857eb44e8ada5e57a595711e9
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08546393B2

연결된 노트

불러오는 중…