Clonidine → 2-[N-(2,6-dichlorophenyl)-N-(2-methyl-1-butene-4-yl)-amino]2-imidazoline

HRID 1277417

反応式

HRID 1277417 の反応式
[CH:1]1[CH:6]=[C:5]([Cl:7])[C:4]([NH:8][C:9]2[NH:13][CH2:12][CH2:11][N:10]=2)=[C:3]([Cl:14])[CH:2]=1.Br[CH2:16][CH2:17][C:18]([CH3:20])=[CH2:19].C(N(CC)CC)C>C1(C)C=CC=CC=1>[Cl:14][C:3]1[CH:2]=[CH:1][CH:6]=[C:5]([Cl:7])[C:4]=1[N:8]([C:9]1[NH:10][CH2:11][CH2:12][N:13]=1)[CH2:16][CH2:17][C:18]([CH3:20])=[CH2:19]

参加物

5

反応物 3

HCID 2803ClonidineHCID 8471TriethylamineHCID 5495854-Bromo-2-methylbut-1-ene

生成物 1

HCID 234541072-[N-(2,6-dichlorophenyl)-N-(2-methyl-1-butene-4-yl)-amino]2-imidazoline

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
120 °C

実験手順

A mixture of 6.9 gm (0.03 mol) of clonidine, 5.6 gm of 4-bromo-2-methyl-1-butene, and 5 ml of triethylamine in 25 ml of toluene was heated for 24 hours at 120° C. After cooling, the solvent was decanted, and the residue remaining was dissolved in 1 N hydrochloric acid. After extraction with ether several times (the ethereal extracts were abandoned), the solution was extracted with ether in fractions at stepwisely rising pH values (alkalizing with 2 N sodium hydroxide solution). The thin-layer chromatographically uniform ether extracts were united and dried over MgSO4, and the ether was evaporated in vacuo.

後処理

  1. temperatureAfter cooling
  2. customthe solvent was decanted
  3. dissolutionthe residue remaining was dissolved in 1 N hydrochloric acid
  4. extractionAfter extraction with ether several times (the ethereal extracts
  5. extractionwas extracted with ether in fractions
  6. dry with materialdried over MgSO4
  7. customthe ether was evaporated in vacuo

出典と根拠

ORDレコード
ord-3d87352bb14d48abb106dbb312628568
出典データセット
uspto-grants-1981_07
特許番号
US04277487

関連ノート

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