Thiophosgene → 2-Tert-butyl-6-isocyanato-5-[4-methyl-piperazin-1-yl]benzothiazole

HRID 2118742

반응식

HRID 2118742 반응식
[NH2:1][C:2]1[C:14]([N:15]2[CH2:20][CH2:19][N:18]([CH3:21])[CH2:17][CH2:16]2)=[CH:13][C:5]2[N:6]=[C:7]([C:9]([CH3:12])([CH3:11])[CH3:10])[S:8][C:4]=2[CH:3]=1.[C:22](=O)(O)[O-:23].[Na+].C(Cl)(Cl)=S.[OH-].[Na+]>C(Cl)(Cl)Cl.O>[C:9]([C:7]1[S:8][C:4]2[CH:3]=[C:2]([N:1]=[C:22]=[O:23])[C:14]([N:15]3[CH2:20][CH2:19][N:18]([CH3:21])[CH2:17][CH2:16]3)=[CH:13][C:5]=2[N:6]=1)([CH3:12])([CH3:11])[CH3:10]

참가 물질

7

반응물 4

HCID 10040ThiophosgeneHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 197941766-Amino-2-tert-butyl-5-(4-methylpiperazin-1-yl)benzothiazole

생성물 1

HCID 201929472-Tert-butyl-6-isocyanato-5-[4-methyl-piperazin-1-yl]benzothiazole

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

To a stirred mixture of 75 g of 6-amino-2-tert-butyl-5-(4-methylpiperazin-1-yl)benzothiazole and 29 g of sodium bicarbonate in 1100 ml of chloroform at 0° is added 41 g of thiophosgene and the mixture stirred at 10° for 4 hours. After filtering off the solid, the solution is evaporated to get an yellow solid which is dissolved in water and the pH of the solution is brought to 7 by the addition of dilute sodium hydroxide. The solid separated is extracted with hexane and filtered through 150 g of neutral alumina to give 2-tert-butyl-6-isocyanato-5-[4-methyl-piperazin-1-yl]benzothiazole melting at 124°-126°.

후처리

  1. filtrationAfter filtering off the solid
  2. customthe solution is evaporated
  3. customto get an yellow solid which
  4. customThe solid separated
  5. extractionis extracted with hexane
  6. filtrationfiltered through 150 g of neutral alumina

출처 및 근거

ORD 기록
ord-d2d22f0b5f2142f4b68d026ed0663809
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04680301

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