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

HRID 2118742

反応式

HRID 2118742 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-d2d22f0b5f2142f4b68d026ed0663809
出典データセット
uspto-grants-1987_07
特許番号
US04680301

関連ノート

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