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

HRID 67644노트

반응식

HRID 67644 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5c6e7c4ddd17458c9b7958e09d737eb1
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04346093

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