Hydrochloric Acid → HCID 67521251、化合物

HRID 1786949ノート

反応式

HRID 1786949 の反応式
C(OC(=O)[NH:7][CH2:8][C:9]1[NH:17][C:16]2[C:15]([NH:18][C:19]3[CH:24]=[CH:23][C:22]([O:25][CH2:26][C:27]4[CH:32]=[CH:31][CH:30]=[C:29]([F:33])[CH:28]=4)=[C:21]([Cl:34])[CH:20]=3)=[N:14][CH:13]=[N:12][C:11]=2[CH:10]=1)(C)(C)C.[ClH:36].C(O)C>O1CCCC1>[ClH:34].[ClH:36].[NH2:7][CH2:8][C:9]1[NH:17][C:16]2[C:15]([NH:18][C:19]3[CH:24]=[CH:23][C:22]([O:25][CH2:26][C:27]4[CH:32]=[CH:31][CH:30]=[C:29]([F:33])[CH:28]=4)=[C:21]([Cl:34])[CH:20]=3)=[N:14][CH:13]=[N:12][C:11]=2[CH:10]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 86626249Carbamic acid, N-[[4-[[3-chloro-4-[(3-fluorophenyl)methoxy]phenyl]amino]-5H-pyrrolo[3,2-d]pyrimidin-6-yl]methyl]-, 1,1-dimethylethyl ester

生成物 1

HCID 67521251HCID 67521251、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

To a solution of tert-butyl[4-({3-chloro-4-[(3-fluorobenzyl)oxy]phenyl}amino)-5H-pyrrolo[3,2-d]pyrimidin-6-yl]methylcarbamate (500 mg) in tetrahydrofuran (12 mL) was added 2N hydrochloric acid (6.0 mL) at room temperature. The mixture was stirred at 60° C. for 2 hrs, ethanol was added to the reaction system and the mixture was concentrated under reduced pressure. The resultant crystals were collected by filtration and washed with diisopropyl ether to give the title compound (481.4 mg) as pale-yellow powder crystals.

後処理

  1. concentrationthe mixture was concentrated under reduced pressure
  2. filtrationThe resultant crystals were collected by filtration
  3. washwashed with diisopropyl ether

出典と根拠

ORDレコード
ord-df99aae6eb6d4398afa663d1b74d2106
出典データセット
uspto-grants-2009_03
特許番号
US07507740B2

反応ノート

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