Triethylamine → 4-(4-Fluoro-3-isocyanato-benzyl)-2H-phthalazin-1-one

HRID 600260

反応式

HRID 600260 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:17]=[CH:18][C:19]=1[F:20])[CH2:5][C:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9](=[O:16])[NH:8][N:7]=1.C(N(CC)CC)C.Cl[C:29](Cl)([O:31]C(=O)OC(Cl)(Cl)Cl)Cl>C(Cl)Cl>[F:20][C:19]1[CH:18]=[CH:17][C:4]([CH2:5][C:6]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9](=[O:16])[NH:8][N:7]=2)=[CH:3][C:2]=1[N:1]=[C:29]=[O:31]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 94429TriphosgeneHCID 184443734-(3-amino-4-fluorobenzyl)-2H-phthalazin-1-one

生成物 1

HCID 598565454-(4-Fluoro-3-isocyanato-benzyl)-2H-phthalazin-1-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a suspension of 4-(3-amino-4-fluoro-benzyl)-2H-phthalazin-1-one (1)(4.0 g, 14.8 mmol) in anhydrous DCM (1.6 L) and triethylamine (4.62 mL, 40.86 mmol), was added a dropwise preformed solution of triphosgene (2.75 g, 9.28 mmol) in anhydrous DCM (327 mL) and stirred for 70 minutes and room temperature. The reaction mixture was then concentrated to dryness in vacuo yielding a grey solid. Single peak in LC-MS analysis, (yield taken to be quantitative) no purification performed. m/z (LC-MS, ESP), RT=4.49 mins, (M+MeOH) 328.0.

後処理

  1. concentrationThe reaction mixture was then concentrated to dryness in vacuo
  2. customyielding a grey solid
  3. customSingle peak in LC-MS analysis, (yield taken to be quantitative)
  4. customno purification

出典と根拠

ORDレコード
ord-78509e2f26d7418f81df896423ac6f67
出典データセット
uspto-grants-2011_03
特許番号
US07902193B2

関連ノート

読み込み中…