Ammonia methanol → HCID 86711293、化合物

HRID 336160ノート

反応式

HRID 336160 の反応式
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

参加物

3

反応物 2

HCID 21705897Ammonia methanolHCID 86711292HCID 86711292、化合物

生成物 1

HCID 86711293HCID 86711293、化合物

反応条件

温度
120 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d2b8c8a4fd9340818430b82963da6b3c
出典データセット
uspto-grants-2014_11
特許番号
US08889666B2

反応ノート

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