Hydrochloric Acid → HCID 67232788, 화합물

HRID 733111노트

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HRID 733111 반응식
[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]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 11611338HCID 11611338, 화합물

생성물 1

HCID 67232788HCID 67232788, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
45 °C

실험 절차

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%)

후처리

  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

출처 및 근거

ORD 기록
ord-a3ad91ba5be84d86a5e42aca7b5db3ba
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07589109B2

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