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

HRID 67102

반응식

HRID 67102 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3ec3306dde864a7c99f123a38144561b
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04344946

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