Lithium hydroxide, monohydrate → HCID 178522632, 화합물

HRID 1035716노트

반응식

HRID 1035716 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[S:12][C:11]([NH:13][C:14]([C:16]3[CH:32]=[CH:31][C:19]([O:20][C@@H:21]4[CH2:26][CH2:25][C@H:24]([C:27]([O:29]C)=[O:28])[CH2:23][CH2:22]4)=[CH:18][CH:17]=3)=[O:15])=[N:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1.O.[OH-].[Li+]>O1CCCC1.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2[S:12][C:11]([NH:13][C:14]([C:16]3[CH:32]=[CH:31][C:19]([O:20][C@@H:21]4[CH2:22][CH2:23][C@H:24]([C:27]([OH:29])=[O:28])[CH2:25][CH2:26]4)=[CH:18][CH:17]=3)=[O:15])=[N:10][N:9]=2)[CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 178501266HCID 178501266, 화합물

생성물 1

HCID 178522632HCID 178522632, 화합물수율 65.5%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

150 mg of methyl cis-4-{4-[5-(3-chlorophenyl)[1.3.4]thiadiazol-2-ylcarbamoyl]phenoxy}-cyclohexanecarboxylate (0.32 mmol, 1 eq.) is placed in 1 mL of tetrahydrofuran. 27 mg of lithium hydroxide monohydrate (0.64 mmol, 2 eq.) dissolved in 1 mL are added and stirring is continued for 18 hours. The reaction medium is diluted with water, washed with ethyl acetate and acidified with aqueous 6% sulfur dioxide solution. The solid obtained is filtered off by suction and washed successively with water, ethanol and diethyl ether. 96 mg of cis-4-{4-[5-(3-chlorophenyl)[1.3.4]thiadiazol-2-ylcarbamoyl]-phenoxy}cyclohexanecarboxylic acid are obtained.

후처리

  1. additionare added
  2. washwashed with ethyl acetate
  3. customThe solid obtained
  4. filtrationis filtered off by suction
  5. washwashed successively with water, ethanol and diethyl ether

출처 및 근거

ORD 기록
ord-6b103727d446442ab4897fec6936ddef
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08546391B2

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