Methyl iodide → HCID 66634917, 화합물

HRID 510070노트

반응식

HRID 510070 반응식
[CH3:1][O:2][C:3]1[CH:38]=[C:37]([O:39][CH3:40])[CH:36]=[CH:35][C:4]=1[CH2:5][N:6]1[C:10]2[N:11]=[C:12]([C:15]3[C:23]4[C:18](=[N:19][CH:20]=[C:21]([F:24])[CH:22]=4)[N:17]([CH2:25][C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=4[F:32])[N:16]=3)[N:13]=[CH:14][C:9]=2[NH:8][S:7]1(=[O:34])=[O:33].[C:41](=O)([O-])[O-].[Cs+].[Cs+].IC>CN(C=O)C>[CH3:1][O:2][C:3]1[CH:38]=[C:37]([O:39][CH3:40])[CH:36]=[CH:35][C:4]=1[CH2:5][N:6]1[C:10]2[N:11]=[C:12]([C:15]3[C:23]4[C:18](=[N:19][CH:20]=[C:21]([F:24])[CH:22]=4)[N:17]([CH2:25][C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=4[F:32])[N:16]=3)[N:13]=[CH:14][C:9]=2[N:8]([CH3:41])[S:7]1(=[O:34])=[O:33]

참가 물질

5

반응물 3

HCID 6328Methyl iodide2회HCID 10796Cesium carbonateHCID 66635554HCID 66635554, 화합물

생성물 1

HCID 66634917HCID 66634917, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

130 mg (approx. 0.115 mmol, 50% purity) of the compound from example 99A were initially charged in 5 ml of DMF, 44 mg (0.138 mmol) of cesium carbonate and 8.5 μl (0.138 mmol) of iodomethane were added and the mixture was stirred at RT overnight. Subsequently, another 14.3 μl (0.230 mmol) of iodomethane were added and the mixture was heated to 50° C. overnight. After cooling, the mixture was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient). This gave 30.9 mg (46% of theory) of the title compound.

후처리

  1. temperaturethe mixture was heated to 50° C. overnight
  2. temperatureAfter cooling
  3. customthe mixture was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient)

출처 및 근거

ORD 기록
ord-ad5d4a5401fd4246bd0f4ec9c0a6c92b
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096592B2

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