Methyl iodide → 1578484-60-2

HRID 523108

반응식

HRID 523108 반응식
[H-].[Na+].[Br:3][C:4]1[CH:5]=[N:6][N:7]([CH3:11])[C:8]=1[CH2:9][OH:10].I[CH3:13]>C1COCC1.CN(C=O)C.C1COCC1.[Cl-].[Na+].O>[Br:3][C:4]1[CH:5]=[N:6][N:7]([CH3:11])[C:8]=1[CH2:9][O:10][CH3:13]

참가 물질

7

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 57415773(4-bromo-1-methyl-1H-pyrazol-5-yl)methanol

생성물 1

HCID 899956041578484-60-2수율 67.2%

시약·촉매·용매 3

HCID 8028Tetrahydrofuran용매HCID 21974620tetrahydrofuran N,N-dimethylformamide용매HCID 57417360Sodium chloride; water용매

실험 절차

NaH (60%, 58 mg) was added to a solution of (4-bromo-1-methyl-1H-pyrazol-5-yl)methanol (Preparation 149, 97 mg, 1.03 mmol) in THF/DMF (8/4 mL). After stirring for 15 minutes, iodomethane (439 mg, 3.09 mmol) in THF (1 mL) was added. The resulting solution was stirred at room temperature for 16 hours. The reaction mixture was diluted with brine and extracted with EtOAc. The combined organic layers were washed with water, dried over sodium sulphate and concentrated in vacuo to afford the title compound (142 mg, 67%).

후처리

  1. stirringThe resulting solution was stirred at room temperature for 16 hours
  2. extractionextracted with EtOAc
  3. washThe combined organic layers were washed with water
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-07e36eea7b7d45ccb68517445ea40eec
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09334286B2

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