2-(beta-Hydroxyethyl)amino-6-(beta-hydroxyethyl)amino-4-chloronitrobenzene → 2-(beta-Hydroxyethyl)amino-6-(beta-hydroxyethyl)amino-4-(beta-aminoethyl)aminonitrobenzene

HRID 1606858노트

반응식

HRID 1606858 반응식
[OH:1][CH2:2][CH2:3][NH:4][C:5]1[CH:10]=[C:9](Cl)[CH:8]=[C:7]([NH:12][CH2:13][CH2:14][OH:15])[C:6]=1[N+:16]([O-:18])=[O:17]>C(N)CN>[OH:1][CH2:2][CH2:3][NH:4][C:5]1[CH:10]=[C:9]([NH:4][CH2:5][CH2:6][NH2:16])[CH:8]=[C:7]([NH:12][CH2:13][CH2:14][OH:15])[C:6]=1[N+:16]([O-:18])=[O:17]

참가 물질

3

반응물 1

HCID 200710912-(beta-Hydroxyethyl)amino-6-(beta-hydroxyethyl)amino-4-chloronitrobenzene

생성물 1

HCID 198511702-(beta-Hydroxyethyl)amino-6-(beta-hydroxyethyl)amino-4-(beta-aminoethyl)aminonitrobenzene

시약·촉매·용매 1

HCID 3301Ethylenediamine용매

실험 절차

0.13 mole (36.5 g) of 2-(β-hydroxyethyl)amino-6-(β-hydroxyethyl)amino-4-chloronitrobenzene, whose synthesis was described in stage 1 of example 2, was heated for 2 hours at 130° C. in 150 ml of ethylenediamine, then the reaction medium diluted with 450 ml of ice water to precipitate out the desired product. After filtering and water washing to neutrality, the product obtained was dried under vacuum in the presence of P2O5. It was recrystallized from 96° ethanol and melted at 220° C.

후처리

  1. customthe reaction
  2. customto precipitate out the desired product
  3. filtrationAfter filtering
  4. customwater washing to neutrality, the product obtained
  5. dry with materialwas dried under vacuum in the presence of P2O5
  6. customIt was recrystallized from 96° ethanol and melted at 220° C.

출처 및 근거

ORD 기록
ord-a1373ab1801340939b767731612b3c47
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04863482

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