Methyl iodide → HCID 68651293、化合物

HRID 2060964ノート

反応式

HRID 2060964 の反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:12](=[CH:13][CH:14]=1)[NH:11][C:10]1[C:9]([O:15][CH2:16][CH2:17][N:18]([CH3:20])[CH3:19])=[C:8]3[NH:21][C:22]4[CH:23]=[CH:24][C:25]([F:28])=[CH:26][C:27]=4[C:7]3=[CH:6][C:5]2=1.[CH3:29][I:30]>ClCCl>[I-:30].[F:28][C:25]1[CH:26]=[C:27]2[C:22](=[CH:23][CH:24]=1)[NH:21][C:8]1[C:9]([O:15][CH2:16][CH2:17][N+:18]([CH3:29])([CH3:19])[CH3:20])=[C:10]3[NH:11][C:12]4[CH:13]=[CH:14][C:2]([F:1])=[CH:3][C:4]=4[C:5]3=[CH:6][C:7]2=1

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 45138929HCID 45138929、化合物

生成物 1

HCID 68651293HCID 68651293、化合物収率 62%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-(2,10-difluoro-5,7-dihydroindolo[2,3-b]carbazol-6-yloxy)-N,N-dimethylethanamine (14 mg) in dichloromethane (8 mL) was added MeI (1.0 mL) at RT under Ar. The resultant solution was stirred overnight and the solid formed. The solid was collected by filtration and washed once with dichloromethane and dried under vacuum to give the title compound (12 mg, 62%). 1H NMR (400 MHz, CD3OD) δ ppm 8.51 (s, 1H), 7.84 (dd, J=9.2, 2.8 Hz, 2H), 7.44 (dd, J=8.8, 4.0 Hz, 2H), 7.12 (ddd, J=9.2, 9.6, 2.4 Hz, 2H), 4.75-4.68 (m, 2H), 4.12-4.07 (m, 2H), 3.46 (s, 9H); MS (ESI) e/z 394 (M−I)+.

後処理

  1. customthe solid formed
  2. filtrationThe solid was collected by filtration
  3. washwashed once with dichloromethane
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-81758a82a9fd4bf19443104f862e7a72
出典データセット
uspto-grants-2012_10
特許番号
US08278341B2

反応ノート

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