Hydrochloric Acid → HCID 67232788、化合物

HRID 733111ノート

反応式

HRID 733111 の反応式
[CH3:1][C:2]1([CH3:30])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]([C:11]([NH:13][CH2:14][CH:15]2[CH2:20][CH2:19][N:18]([CH2:21][C:22]3([C:26]([OH:28])=[O:27])[CH2:25][CH2:24][CH2:23]3)[CH2:17][CH2:16]2)=[O:12])[C:3]1=[O:29].[ClH:31]>O1CCCC1>[ClH:31].[CH3:1][C:2]1([CH3:30])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]([C:11]([NH:13][CH2:14][CH:15]2[CH2:20][CH2:19][N:18]([CH2:21][C:22]3([C:26]([OH:28])=[O:27])[CH2:25][CH2:24][CH2:23]3)[CH2:17][CH2:16]2)=[O:12])[C:3]1=[O:29]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 11611338HCID 11611338、化合物

生成物 1

HCID 67232788HCID 67232788、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
45 °C

実験手順

1-{[4-({[(3,3-Dimethyl-2-oxo-2,3-dihydro-1h-indol-1-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}cyclobutanecarboxylic acid (41.0 g, 99.2 mmol, Example 9) was dissolved with tetrahydrofuran (820 mL). The mixture was filtered and washed with tetrahydrofuran (410 mL) and the resulting solution was heated to 45° C. Aqueous concentrated hydrogen chloride (12N, 8.27 mL, 99.2 mmol) was added to the solution at 45° C. for 20 min and stirred at this temperature for 1 h. The suspension was cooled to 20° C. for 1 min stirred at 2 h. After filtration, the resulting solid was washed with tetrahydrofuran (205 mL), and dried in vacuo at 40° C. The titled compound was obtained as white solid (38.6 g, 86.6%)

後処理

  1. filtrationThe mixture was filtered
  2. washwashed with tetrahydrofuran (410 mL)
  3. temperatureThe suspension was cooled to 20° C. for 1 min
  4. stirringstirred at 2 h
  5. filtrationAfter filtration
  6. washthe resulting solid was washed with tetrahydrofuran (205 mL)
  7. customdried in vacuo at 40° C

出典と根拠

ORDレコード
ord-a3ad91ba5be84d86a5e42aca7b5db3ba
出典データセット
uspto-grants-2009_09
特許番号
US07589109B2

反応ノート

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