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

HRID 600260노트

반응식

HRID 600260 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-78509e2f26d7418f81df896423ac6f67
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902193B2

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