HCID 86655023, 화합물 → HCID 58333381, 화합물

HRID 2066892노트

반응식

HRID 2066892 반응식
[F:1][C:2]1[CH:7]=[C:6]([S:8]([CH3:11])(=[O:10])=[O:9])[CH:5]=[CH:4][C:3]=1[N:12]1[CH2:17][CH2:16][C:15](=[N:18][O:19][CH:20]2[CH2:25][CH2:24][N:23]([C:26]#[N:27])[CH2:22][CH2:21]2)[CH2:14][CH2:13]1.[OH:28][NH:29][C:30](=N)[CH:31]([CH3:33])[CH3:32]>C(OCC)(=O)C.[Cl-].[Cl-].[Zn+2]>[CH:31]([C:30]1[N:27]=[C:26]([N:23]2[CH2:24][CH2:25][CH:20]([O:19][N:18]=[C:15]3[CH2:16][CH2:17][N:12]([C:3]4[CH:4]=[CH:5][C:6]([S:8]([CH3:11])(=[O:9])=[O:10])=[CH:7][C:2]=4[F:1])[CH2:13][CH2:14]3)[CH2:21][CH2:22]2)[O:28][N:29]=1)([CH3:33])[CH3:32]

참가 물질

5

반응물 2

HCID 86655023HCID 86655023, 화합물HCID 178449908HCID 178449908, 화합물

생성물 1

HCID 58333381HCID 58333381, 화합물

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 8857Ethyl Acetate용매

실험 절차

68b (35 mg, 0.066 mmol) and 68a (8 mg, 0.08 mmol) were combined in ethyl acetate (1 mL) and 1N ZnCl2 (80 μL, 0.08 mmol) was added dropwise. After 1 h, the solvent was evaporated. 1 mL of ethanol and 0.5 mL of concentrated HCl were added and the mixture was heated to reflux. The solvent was removed and the crude mixture was purified on preparative HPLC to give 68-1: LC-MS 480.2 (MH+), tR=5.57 (Method 5).

후처리

  1. customthe solvent was evaporated
  2. addition1 mL of ethanol and 0.5 mL of concentrated HCl were added
  3. temperaturethe mixture was heated to reflux
  4. customThe solvent was removed
  5. customthe crude mixture was purified on preparative HPLC
  6. customto give 68-1

출처 및 근거

ORD 기록
ord-48cb117126574275b474e7ed042c68b9
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293729B2

반응 노트

불러오는 중…