Sodium Hydroxide → [4-(1-Methylpiperidin-4-ylidene)-4,10-dihydro-9-oxa-3-thiabenzo[f]azulen-6-ylsulfanyl]acetic acid

HRID 389033노트

반응식

HRID 389033 반응식
[OH-].[Na+].C[O:4][C:5](=[O:29])[CH2:6][S:7][C:8]1[CH:9]=[CH:10][C:11]2[O:20][CH2:19][C:18]3[CH:17]=[CH:16][S:15][C:14]=3[CH:13]([CH:21]3[CH2:26][CH2:25][N:24]([CH3:27])[CH2:23][CH2:22]3)[C:12]=2[CH:28]=1>C(O)C>[CH3:27][N:24]1[CH2:25][CH2:26][C:21](=[C:13]2[C:12]3[CH:28]=[C:8]([S:7][CH2:6][C:5]([OH:29])=[O:4])[CH:9]=[CH:10][C:11]=3[O:20][CH2:19][C:18]3[CH:17]=[CH:16][S:15][C:14]2=3)[CH2:22][CH2:23]1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 86649444Methyl[4-(1-methylpiperidin-4-yl)-4,10-dihydro-9-oxa-3-thiabenzo[f]azulen-6-ylsulfanyl]acetate

생성물 1

HCID 68490446[4-(1-Methylpiperidin-4-ylidene)-4,10-dihydro-9-oxa-3-thiabenzo[f]azulen-6-ylsulfanyl]acetic acid수율 50.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

An aqueous sodium hydroxide (1.4 g, 680 mmol) solution was added to an ethanol (40 mL) solution of the compound obtained in Example 24 (2.9 g, 6.7 mmol), and the mixture was refluxed while heating for 2 hours. After allowing the mixture to cool in the air, the solvents were distilled off under a reduced pressure, water was added to the residue, and the mixture was neutralized with hydrochloric acid. The precipitated crystals were separated by filtration and dried, to give 1.3 g (50%) of the captioned compound.

후처리

  1. temperaturethe mixture was refluxed
  2. temperaturewhile heating for 2 hours
  3. temperatureto cool in the air
  4. distillationthe solvents were distilled off under a reduced pressure, water
  5. additionwas added to the residue
  6. customThe precipitated crystals were separated by filtration
  7. customdried

출처 및 근거

ORD 기록
ord-db03ff07f27a4a339233a45dfa203a32
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08377967B2

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