Hydrochloric Acid → HCID 67521251、化合物

HRID 1926036ノート

反応式

HRID 1926036 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:17][C:18]2[C:19]3[NH:26][C:25]([CH2:27][NH:28]C(=O)OC(C)(C)C)=[CH:24][C:20]=3[N:21]=[CH:22][N:23]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=1.[ClH:36].C(O)C>O1CCCC1>[ClH:1].[ClH:36].[NH2:28][CH2:27][C:25]1[NH:26][C:19]2[C:18]([NH:17][C:4]3[CH:5]=[CH:6][C:7]([O:8][CH2:9][C:10]4[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=4)=[C:2]([Cl:1])[CH:3]=3)=[N:23][CH:22]=[N:21][C:20]=2[CH:24]=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-30aea98815ec4dfab332a9050ef94603
出典データセット
uspto-grants-2012_05
特許番号
US08178543B2

反応ノート

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