Hydrochloric Acid → Camptosar

HRID 2115184

反応式

HRID 2115184 の反応式
[CH3:1][CH2:2][C:3]1[C:12]2[CH2:13][N:14]3[C:19](=[O:20])[C:18]4[CH2:21][O:22][C:23]([C@:25]([OH:28])([CH2:26][CH3:27])[C:17]=4[CH:16]=[C:15]3[C:11]=2[N:10]=[C:9]2[C:4]=1[CH:5]=[C:6]([O:29][C:30]([N:32]1[CH2:37][CH2:36][CH:35]([N:38]3[CH2:43][CH2:42][CH2:41][CH2:40][CH2:39]3)[CH2:34][CH2:33]1)=[O:31])[CH:7]=[CH:8]2)=[O:24].C([O-])(=[O:46])C.C[OH:49].[ClH:50]>C(OCC)(=O)C>[CH3:1][CH2:2][C:3]1[C:12]2[CH2:13][N:14]3[C:19](=[O:20])[C:18]4[CH2:21][O:22][C:23]([C@:25]([OH:28])([CH2:26][CH3:27])[C:17]=4[CH:16]=[C:15]3[C:11]=2[N:10]=[C:9]2[C:4]=1[CH:5]=[C:6]([O:29][C:30]([N:32]1[CH2:33][CH2:34][CH:35]([N:38]3[CH2:43][CH2:42][CH2:41][CH2:40][CH2:39]3)[CH2:36][CH2:37]1)=[O:31])[CH:7]=[CH:8]2)=[O:24].[OH2:46].[OH2:49].[OH2:20].[ClH:50]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 131727091Irinotecan acetate

生成物 1

HCID 60837Camptosar

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

To a 100 mL reactor was charged amorphous irinotecan acetate (2.0 g) and methanol (14 mL). The reaction mixture was heated to 50° C. 2N hydrochloric acid (6.2 wt %, about 1.7 mL) was added to adjust the pH level to less than 4 in order to dissolve the solid particles. Ethyl acetate (40 mL) was added slowly to the mixture. The mixture was cooled to 0˜10° C. and stirred at this temperature for 1 hour. The solid particles were filtered and washed with cooled ethyl acetate (6 mL). The wet cake was dried in vacuum to give 1.66 g of irinotecan hydrochloride trihydrate Form III.

後処理

  1. dissolutionto dissolve the solid particles
  2. temperatureThe mixture was cooled to 0˜10° C.
  3. filtrationThe solid particles were filtered
  4. washwashed with cooled ethyl acetate (6 mL)
  5. customThe wet cake was dried in vacuum

出典と根拠

ORDレコード
ord-2aa15cc8bbfe45299c8161d26930e368
出典データセット
uspto-grants-2008_10
特許番号
US07435818B2

関連ノート

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