Ammonium Chloride → 10-Chloro-2-iodo-5,6-dihydroimidazo[1,2-d]pyrido[4,3-f][1,4]oxazepine

HRID 886023노트

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HRID 886023 반응식
C([Mg]Cl)(C)C.[Cl:6][C:7]1[N:17]=[CH:16][C:15]2[O:14][CH2:13][CH2:12][N:11]3[C:18](I)=[C:19]([I:21])[N:20]=[C:10]3[C:9]=2[CH:8]=1.[NH4+].[Cl-]>O1CCCC1>[Cl:6][C:7]1[N:17]=[CH:16][C:15]2[O:14][CH2:13][CH2:12][N:11]3[CH:18]=[C:19]([I:21])[N:20]=[C:10]3[C:9]=2[CH:8]=1

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 5820465310-Chloro-2,3-diiodo-5,6-dihydroimidazo[1,2-d]pyrido[4,3-f][1,4]oxazepineHCID 178418918HCID 178418918, 화합물

생성물 1

HCID 5820436210-Chloro-2-iodo-5,6-dihydroimidazo[1,2-d]pyrido[4,3-f][1,4]oxazepine수율 98.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
10 °C

실험 절차

Isopropylmagnesium chloride in tetrahydrofuran (2.0 M, 3.311 mL) was added dropwise to a solution of 10-chloro-2,3-diiodo-5,6-dihydroimidazo[1,2-d]pyrido[4,3-f][1,4]oxazepine (2.850 g, 6.020 mmol) in 110 ml of tetrahydrofuran at −10° C. The mixture was allowed to warm to 10° C. in 45 min and then mixed with 250 ml of cold 10% NH4Cl. The organic layer was washed with brine and dried over Na2SO4. Concentration in vacuum afforded 2.06 g of 10-chloro-2-iodo-5,6-dihydroimidazo[1,2-d]pyrido[4,3-f][1,4]oxazepine (98.5%). MS: 348.0. 1H NMR (500 MHz, CDCl3) δ 8.33 (d, J=10.1, 1H), 8.18 (s, 1H), 7.18 (s, 1H), 4.46 (q, J=5.8, 4H).

후처리

  1. washThe organic layer was washed with brine
  2. dry with materialdried over Na2SO4
  3. concentrationConcentration in vacuum

출처 및 근거

ORD 기록
ord-d68c2d494c5b4583add6bc0915c60f9f
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08242104B2

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