1-Chloroethyl chloroformate → 2-bromo-N-methyl-N-(1-methylethyl)-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine hydrochloride

HRID 1879770노트

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HRID 1879770 반응식
C([N:8]1[CH2:14][C:13]2[N:15]=[C:16]([Br:24])[C:17]([N:19]([CH3:23])[CH:20]([CH3:22])[CH3:21])=[N:18][C:12]=2[O:11][CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:25]C(OC(Cl)C)=O>C1(C)C=CC=CC=1>[ClH:25].[Br:24][C:16]1[C:17]([N:19]([CH3:23])[CH:20]([CH3:21])[CH3:22])=[N:18][C:12]2[O:11][CH2:10][CH2:9][NH:8][CH2:14][C:13]=2[N:15]=1

참가 물질

4

반응물 2

HCID 5213051-Chloroethyl chloroformateHCID 866490048-benzyl-2-bromo-N-methyl-N-(1-methylethyl)-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine

생성물 1

HCID 866490142-bromo-N-methyl-N-(1-methylethyl)-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine hydrochloride수율 56%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
80 °C

실험 절차

To a solution of 8-benzyl-2-bromo-N-methyl-N-(1-methylethyl)-6,7,8,9-tetrahydropyrazino[2,3-f][1,4]oxazepin-3-amine (122 mg) in toluene (2 mL) was added 1-chloroethyl chloroformate (0.040 mL), and the mixture was stirred at 80° C. for 2 hr. The reaction mixture was cooled to room temperature, and concentrated. To the obtained residue was added methanol (2 mL), and the mixture was stirred at 80° C. for 1 hr. The reaction mixture was cooled to room temperature, and concentrated. The obtained residue was purified by recrystallization (methanol-diisopropyl ether) to give the title compound (59 mg, 56%) as pale-yellow crystals.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationconcentrated
  3. additionTo the obtained residue was added methanol (2 mL)
  4. stirringthe mixture was stirred at 80° C. for 1 hr
  5. temperatureThe reaction mixture was cooled to room temperature
  6. concentrationconcentrated
  7. customThe obtained residue was purified by recrystallization (methanol-diisopropyl ether)

출처 및 근거

ORD 기록
ord-0f460173d84c43e995c57c04711d09ed
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318722B2

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