Hydrochloric Acid → Unii-25K23E3mnm

HRID 1595176ノート

反応式

HRID 1595176 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:26]=[CH:27][C:28]=1[O:29][CH3:30])[CH2:5][NH:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:17]#[N:18])[CH:15]=2)[C:10]([N:19]2[CH2:24][CH2:23][CH:22]([OH:25])[CH2:21][CH2:20]2)=[N:9][N:8]=1.O.Cl>C(O)C>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([CH:26]=[CH:27][C:28]=1[O:29][CH3:30])[CH2:5][NH:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([C:17]#[N:18])[CH:15]=2)[C:10]([N:19]2[CH2:20][CH2:21][CH:22]([OH:25])[CH2:23][CH2:24]2)=[N:9][N:8]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 9888568Yze9gcm2BB

生成物 1

HCID 9955887Unii-25K23E3mnm収率 159.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

10.8 g of 4-(3-chloro-4-methoxybenzyl)amino-6-cyano-1-(4-hydroxypiperidino)phthalazine was suspended in a mixture of ethanol (60 ml) with water (30 ml) and 30 ml of a 1 N aqueous solution of hydrochloric acid was added thereto. After dissolving by heating once, the mixture was cooled by allowing to stand at room temperature. The resulting crystals were collected by filtration and hot air-dried at 80° C. overnight to give 9.37 g of the title compound as yellow crystals. M.p. 217-227° C. (decomp.), Mass 424 (MH+),

後処理

  1. additionwas added
  2. dissolutionAfter dissolving
  3. temperatureby heating once
  4. temperaturethe mixture was cooled
  5. customto stand at room temperature
  6. filtrationThe resulting crystals were collected by filtration
  7. customhot air-dried at 80° C. overnight

出典と根拠

ORDレコード
ord-0b8b46a09c424f3b8626ef142c19fd1e
出典データセット
uspto-grants-2001_09
特許番号
US06288064B1

反応ノート

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