Triethylamine → Nictiazem

HRID 464244노트

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HRID 464244 반응식
[CH3:1][N:2]([CH3:26])[CH2:3][CH2:4][N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[S:9][C@@H:8]([C:16]2[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=2)[C@@H:7]([OH:24])[C:6]1=[O:25].C(N(CC)CC)C.[C:34](Cl)(=[O:41])[C:35]1[CH:40]=[CH:39][CH:38]=[N:37][CH:36]=1>C1C=CC=CC=1>[CH3:26][N:2]([CH3:1])[CH2:3][CH2:4][N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[S:9][C@@H:8]([C:16]2[CH:17]=[CH:18][C:19]([O:22][CH3:23])=[CH:20][CH:21]=2)[C@@H:7]([O:24][C:34](=[O:41])[C:35]2[CH:40]=[CH:39][CH:38]=[N:37][CH:36]=2)[C:6]1=[O:25]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 82604Nicotinoyl chlorideHCID 91638Deacetyldiltiazem

생성물 1

HCID 10457747Nictiazem

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

7 Grams (0.0188 mole) of the compound prepared under (A) were dissolved in 80 ml of anhydrous benzene, and the resulting solution was added with 8 ml (0.0574 mole) of triethylamine and 5 g (0.0281 mole) of nicotinoylchloride suspended in 20 ml of anhydrous benzene. The reaction mixture was heated for 24 hours on an oil bath at 55°-60° C. under stirring then, after cooling, it was twice washed with water and the organic phase was dried over sodium sulfate. The organic solvent was removed in vacuo until formation of a precipitate then, after complete precipitation, the obtained solid was recovered by filtration, washed with anhydrous diethyl ether and dried overnight at 70° C.

후처리

  1. temperatureThe reaction mixture was heated for 24 hours on an oil bath at 55°-60° C.
  2. temperatureafter cooling
  3. washit was twice washed with water
  4. dry with materialthe organic phase was dried over sodium sulfate
  5. customThe organic solvent was removed in vacuo until formation of a precipitate
  6. customafter complete precipitation
  7. filtrationthe obtained solid was recovered by filtration
  8. washwashed with anhydrous diethyl ether
  9. customdried overnight at 70° C.

출처 및 근거

ORD 기록
ord-f625e0a9cf6c4a8faa764f1af7128819
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04547495

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