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Imidazole → HCID 59543005, 화합물

HRID 1876337
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HRID 1876337 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([NH:11][CH:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)[CH:10]=1)[NH:7][C:6]([C:18]1[S:19][CH2:20][C@@H:21]([CH2:23][CH2:24]O)[N:22]=1)=[CH:5]2.N1C=CN=C1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[I:50]I>O1CCCC1.C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([NH:11][CH:12]3[CH2:17][CH2:16][O:15][CH2:14][CH2:13]3)[CH:10]=1)[NH:7][C:6]([C:18]1[S:19][CH2:20][C@@H:21]([CH2:23][CH2:24][I:50])[N:22]=1)=[CH:5]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 795ImidazoleHCID 807IodineHCID 11776TriphenylphosphineHCID 25196937HCID 25196937, 화합물

생성물 1

HCID 59543005HCID 59543005, 화합물수율 40%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매
HCID 8857
Ethyl Acetate
용매

실험 절차

The compound (3.7 g, 10.2 mmol) prepared in Example 32 was dissolved in tetrahydrofuran (100 ml). Imidazole (2.1 g, 30.6 mmol), triphenylphosphine (4.0 g, 15.3 mmol), and iodine (3.9 g, 15.3 mmol) were added thereto, and the mixture was stirred for 8 h at 0° C.˜room temperature. After completion of the reaction, ethyl acetate (100 ml) was added, and the mixture was washed with water (2×100 ml). The organic layer was concentrated, and the residue was separated by column chromatography to give the title compound (2.0 g, 4.07 mmol, Yield 40%).

후처리

  1. additionwas added
  2. washthe mixture was washed with water (2×100 ml)
  3. concentrationThe organic layer was concentrated
  4. customthe residue was separated by column chromatography

출처 및 근거

ORD 기록
ord-56358d159bec4bcaac345a8c8b772dd7
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08309586B2

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