Water → 2,6-Bis-(diethylaminoacetylamino)-benzo[1,2-d:5,4-d']bisthiazole

HRID 67102

反応式

HRID 67102 の反応式
C(N=C=NC[CH2:7][CH2:8][N:9]([CH2:12][CH3:13])[CH2:10][CH3:11])C.[NH2:14][C:15]1[S:16][C:17]2[C:18](=[CH:20][C:21]3[N:22]=[C:23]([NH2:27])[S:24][C:25]=3[CH:26]=2)[N:19]=1.[CH2:28]([N:30]([CH2:35][CH3:36])[CH2:31][C:32](O)=[O:33])[CH3:29].[OH2:37]>C(Cl)Cl>[CH2:28]([N:30]([CH2:31][C:32]([NH:27][C:23]1[S:24][C:25]2[C:21](=[CH:20][C:18]3[N:19]=[C:15]([NH:14][C:7](=[O:37])[CH2:8][N:9]([CH2:12][CH3:13])[CH2:10][CH3:11])[S:16][C:17]=3[CH:26]=2)[N:22]=1)=[O:33])[CH2:35][CH3:36])[CH3:29]

参加物

6

反応物 4

HCID 962WaterHCID 74151N,N-DiethylglycineHCID 844005ST076754HCID 99645131-Ethyl-3-(3-diethylaminopropyl)carbodiimide

生成物 1

HCID 151799672,6-Bis-(diethylaminoacetylamino)-benzo[1,2-d:5,4-d']bisthiazole

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1.0 gm of ethyl-3-(3-diethylamino-propyl)-carbodiimide was added to a suspension of 555 mgm of 2,6-diamino-benzo[1,2-d:5,4-d']bisthiazole and 655 mgm of N,N-diethyl-glycine in 20 ml of methylene chloride, and the mixture was stirred overnight at room temperature. After adding water and filtering off the precipitate, the methylene chloride phase was separated, dried, concentrated and chromatographed on a dry 10 gm-silicagel column with chloroform as the mobile phase. The title compound was collected in the first fractions and converted into the dihydrochloride by treatment with ethereal hydrochloric acid.

後処理

  1. filtrationfiltering off the precipitate
  2. customthe methylene chloride phase was separated
  3. customdried
  4. concentrationconcentrated
  5. customchromatographed on a dry 10 gm-silicagel column with chloroform as the mobile phase
  6. customThe title compound was collected in the first fractions

出典と根拠

ORDレコード
ord-3ec3306dde864a7c99f123a38144561b
出典データセット
uspto-grants-1982_08
特許番号
US04344946

関連ノート

読み込み中…