Ethanol hydrochloride → 2-Cyclopropyl-7-[(3s)-3-(dimethylamino)pyrrolidin-1-yl]-6-formyl-5-methyl-1,3-benzoxazole-4-carbonitrile hydrochloride

HRID 17462

반응식

HRID 17462 반응식
[CH:1]1([C:4]2[O:5][C:6]3[C:7](=[C:9]([C:24]#[N:25])[C:10]([CH3:23])=[C:11]([CH:21]=[O:22])[C:12]=3[N:13]3[CH2:17][CH2:16][C@H:15]([N:18]([CH3:20])[CH3:19])[CH2:14]3)[N:8]=2)[CH2:3][CH2:2]1.[ClH:26].C(O)C>C(O)C.C(OCC)C>[ClH:26].[CH:1]1([C:4]2[O:5][C:6]3[C:7](=[C:9]([C:24]#[N:25])[C:10]([CH3:23])=[C:11]([CH:21]=[O:22])[C:12]=3[N:13]3[CH2:17][CH2:16][C@H:15]([N:18]([CH3:20])[CH3:19])[CH2:14]3)[N:8]=2)[CH2:2][CH2:3]1

참가 물질

5

반응물 2

HCID 21887872Ethanol hydrochlorideHCID 866308522-Cyclopropyl-7-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-formyl-5-methyl-1,3-benzoxazole-4-carbonitrile

생성물 1

HCID 875066112-Cyclopropyl-7-[(3s)-3-(dimethylamino)pyrrolidin-1-yl]-6-formyl-5-methyl-1,3-benzoxazole-4-carbonitrile hydrochloride

시약·촉매·용매 2

HCID 702Ethanol용매HCID 3283Diethyl Ether용매

실험 절차

The above-obtained 2-cyclopropyl-7-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-formyl-5-methyl-1,3-benzoxazole-4-carbonitrile (50 mg, 0.15 mmol) was dissolved in ethanol (0.5 ml) and diethyl ether (1 ml), then at room temperature, 1 mol hydrochloric acid/ethanol solution (162 μl, 0.16 mmol) was added. After stirring under nitrogen atmosphere at the same temperature for 3 hours, the solvent was evaporated away under reduced pressure. Diethyl ether was added to the residue, and this was concentrated under reduced pressure. This operation was repeated further twice.

후처리

  1. customthe solvent was evaporated away under reduced pressure
  2. additionDiethyl ether was added to the residue
  3. concentrationthis was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-2a61c6f12b354501a8bb69fbf7daa579
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737166B2

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