Acetic Acid → 4-[2-Hydroxy-3-(3,4-dimethoxyphenethylamino)-propoxy]-benzotriazole hydrochloride

HRID 67644ノート

反応式

HRID 67644 の反応式
[ClH:1].Cl.Cl.[NH2:4][C:5]1[C:10]([NH2:11])=[CH:9][CH:8]=[CH:7][C:6]=1[O:12][CH2:13][CH:14]([OH:29])[CH2:15][NH:16][CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[C:21]([O:27][CH3:28])[CH:20]=1.C(O)(=O)C.[N:34]([O-])=O.[Na+]>O>[ClH:1].[OH:29][CH:14]([CH2:15][NH:16][CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[C:21]([O:27][CH3:28])[CH:20]=1)[CH2:13][O:12][C:6]1[C:5]2[N:4]=[N:34][NH:11][C:10]=2[CH:9]=[CH:8][CH:7]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 205275092,3-Diamino-1-[2-hydroxy-3-(3,4-dimethoxyphenethylamino)-propoxy]-benzene trihydrochlorideHCID 23668193Sodium Nitrite

生成物 1

HCID 1784903364-[2-Hydroxy-3-(3,4-dimethoxyphenethylamino)-propoxy]-benzotriazole hydrochloride

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

14.1 g. 2,3-Diamino-1-[2-hydroxy-3-(3,4-dimethoxyphenethylamino)-propoxy]-benzene trihydrochloride are dissolved in 10 ml. water and 3.5 ml. glacial acetic acid, cooled to 5° C. and mixed with 2.07 g. sodium nitrite in 3.6 ml. water. The reaction mixture is then stirred for 2.5 hours at ambient temperature. The resultant sodium chloride is precipitated out by the addition of 480 ml. isopropanol. After filtration, the filtrate is evaporated, purified over a column of silica gel using methanol/ethyl acetate (2:1 v/v) as elution agent, mixed with ethereal hydrochloric acid and the hydrochloride so obtained is crystallized from ethanol. There are obtained 1.26 g. (10% of theory) 4-[2-hydroxy-3-(3,4-dimethoxyphenethylamino)-propoxy]-benzotriazole hydrochloride; m.p. 123°-124° C.

後処理

  1. additionmixed with 2.07 g
  2. customThe resultant sodium chloride is precipitated out by the addition of 480 ml
  3. filtrationAfter filtration
  4. customthe filtrate is evaporated
  5. custompurified over a column of silica gel
  6. washas elution agent
  7. additionmixed with ethereal hydrochloric acid

出典と根拠

ORDレコード
ord-5c6e7c4ddd17458c9b7958e09d737eb1
出典データセット
uspto-grants-1982_08
特許番号
US04346093

反応ノート

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