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Benzoyl chloride → 1-(benzoyloxymethyl)-9,10-dimethoxy-1,6,7,11b-tetrahydro-2H,4H-[1,3]oxazino-[4,3-a]isoquinoline

HRID 1731736
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HRID 1731736 반응식
[OH:1][CH2:2][CH:3]1[CH:8]2[C:9]3[C:14]([CH2:15][CH2:16][N:7]2[CH2:6][O:5][CH2:4]1)=[CH:13][C:12]([O:17][CH3:18])=[C:11]([O:19][CH3:20])[CH:10]=3.[C:21](Cl)(=[O:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>N1C=CC=CC=1>[C:21]([O:1][CH2:2][CH:3]1[CH:8]2[C:9]3[C:14]([CH2:15][CH2:16][N:7]2[CH2:6][O:5][CH2:4]1)=[CH:13][C:12]([O:17][CH3:18])=[C:11]([O:19][CH3:20])[CH:10]=3)(=[O:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1
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참가 물질

4

반응물 2

HCID 7412Benzoyl chlorideHCID 145953501-(hydroxymethyl)-9,10-dimethoxy-1,6,7,11b-tetrahydro-2H,4H-[1,3]oxazino[4,3-a]isoquinoline

생성물 1

HCID 145953651-(benzoyloxymethyl)-9,10-dimethoxy-1,6,7,11b-tetrahydro-2H,4H-[1,3]oxazino-[4,3-a]isoquinoline수율 55%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

0.01 mole (2.79 g) of 1-(hydroxymethyl)-9,10-dimethoxy-1,6,7,11b-tetrahydro-2H,4H-[1,3]oxazino[4,3-a]isoquinoline in 30 ml of absolute pyridine is boiled with 0.012 mole (1.69 g) of benzoyl chloride for 3 hours. The mixture is then poured onto 100 g of ice. The separated crystals are filtered off, washed with water and recrystallized from a mixture of diisopropyl ether and ethanol. Yield: 55%. The melting point and spectroscopical data of the compound are identical with those of the product obtained in Example 25.

후처리

  1. filtrationThe separated crystals are filtered off
  2. washwashed with water
  3. customrecrystallized from a mixture of diisopropyl ether and ethanol

출처 및 근거

ORD 기록
ord-acf5eb8389604fd994c8f273983a2481
출처 데이터셋
uspto-grants-1986_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04623647

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