Tetrahydrofuran → HCID 86664952, 화합물

HRID 74291노트

반응식

HRID 74291 반응식
Cl.[NH2:2][CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][C:12]([C:14]3[O:15][C:16]4[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=4[N:18]=3)=[CH:13][C:8]=2[N:7]=[C:6]1[CH3:23].[CH3:24][N:25]=[C:26]=[S:27].C(N(CC)CC)C.C1COCC1>O.C(Cl)(Cl)Cl>[O:15]1[C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[N:18]=[C:14]1[C:12]1[CH:11]=[CH:10][C:9]2[N:5]([CH2:4][CH2:3][NH:2][C:26](=[S:27])[NH:25][CH3:24])[C:6]([CH3:23])=[N:7][C:8]=2[CH:13]=1

참가 물질

7

반응물 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 11167Methyl isothiocyanateHCID 674977031-(2-Aminoethyl)-5-(benzoxazol-2-yl)-2-methylbenzimidazole hydrochloride

생성물 1

HCID 86664952HCID 86664952, 화합물수율 40%

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

1-(2-Aminoethyl)-5-(benzoxazol-2-yl)-2-methylbenzimidazole hydrochloride (see Working Example 56) (0.20 g, 0.6 mmol), methyl isothiocyanate (0.17 g, 0.6 mmol), triethylamine (0.13 g, 13 mmol) and THF (2 mL) were added together, and stirred for 1 hour at room temperature. After cooling, chloroform and water were added and extraction was carried out. After the organic layer obtained was dried over anhydrous sodium sulfate, it was filtered and concentrated. The solid obtained was separated by filtration and dried to yield the title compound (0.08 g, 40% yield) as white crystals.

후처리

  1. temperatureAfter cooling
  2. extractionextraction
  3. customAfter the organic layer obtained
  4. dry with materialwas dried over anhydrous sodium sulfate, it
  5. filtrationwas filtered
  6. concentrationconcentrated
  7. customThe solid obtained
  8. customwas separated by filtration
  9. customdried

출처 및 근거

ORD 기록
ord-2a8d93b5a41341c3a3b0bf5871e0ab9f
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829035B2

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