Ammonia methanol → HCID 86711293, 화합물

HRID 336160노트

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HRID 336160 반응식
CO.[NH3:3].Cl[C:5]1[C:6]2[C:13]([I:14])=[CH:12][N:11]([CH2:15][C@@H:16]([NH:19][C:20](=[O:26])[O:21][C:22]([CH3:25])([CH3:24])[CH3:23])[CH:17]=[CH2:18])[C:7]=2[N:8]=[CH:9][N:10]=1>>[NH2:3][C:5]1[C:6]2[C:13]([I:14])=[CH:12][N:11]([CH2:15][C@@H:16]([NH:19][C:20](=[O:26])[O:21][C:22]([CH3:25])([CH3:24])[CH3:23])[CH:17]=[CH2:18])[C:7]=2[N:8]=[CH:9][N:10]=1

참가 물질

3

반응물 2

HCID 21705897Ammonia methanolHCID 86711292HCID 86711292, 화합물

생성물 1

HCID 86711293HCID 86711293, 화합물

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온도
120 °C

실험 절차

An 8 N ammonia methanol solution (89.4 ml) was added to the (S)-tert-butyl (1-(4-chloro-5-iodo-7H-pyrrolo[2,3-d]pyrimidin-7-yl)but-3-en-2-yl)carbamate (20.84 g) obtained in Step 1, and the mixture was stirred in an autoclave at 120° C. for 6 hours. The reaction mixture was cooled with ice, and the solvent was distilled off under reduced pressure. After the resulting residue was diluted with a small amount of methanol, the resulting precipitate was collected by filtration, washed with cold methanol (11 ml), and then dried under reduced pressure to obtain the title compound (8.28 g) as a milky-white solid.

후처리

  1. temperatureThe reaction mixture was cooled with ice
  2. distillationthe solvent was distilled off under reduced pressure
  3. additionAfter the resulting residue was diluted with a small amount of methanol
  4. filtrationthe resulting precipitate was collected by filtration
  5. washwashed with cold methanol (11 ml)
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-d2b8c8a4fd9340818430b82963da6b3c
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889666B2

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