Potassium Carbonate → 4-[(1H-1,3-benzodiazol-2-ylsulfanyl)methyl]benzoic acid

HRID 34671

반응식

HRID 34671 반응식
[SH:1][C:2]1[NH:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.C([O-])([O-])=O.[K+].[K+].Br[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]([OH:27])=[O:26])=[CH:21][CH:20]=1>CN(C=O)C>[C:25]([C:22]1[CH:23]=[CH:24][C:19]([CH2:18][S:1][C:2]2[NH:3][C:4]3[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=3[N:6]=2)=[CH:20][CH:21]=1)([OH:27])=[O:26]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 225994-(Bromomethyl)benzoic acidHCID 178527775HCID 178527775, 화합물

생성물 1

HCID 49921594-[(1H-1,3-benzodiazol-2-ylsulfanyl)methyl]benzoic acid

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

4.6 g (30 mmol) of 2-mercaptobenzimidazole were initially introduced into 60 ml of dry DMF, 8.3 g (60 mmol) of K2CO3 were added, and a solution of 6.7 g (31 mmol) of α-bromo-4-toluic acid in 15 ml of dry DMF was added dropwise at room temperature. After 4 hours, a solid residue was filtered off with suction, the DMF was removed in vacuo, and the residue was taken up in aqueous hydrochloric acid at pH 2. Crystals of the title compound separated out, and these were washed with water, methanol and ether and dried.

후처리

  1. additionwere added
  2. filtrationa solid residue was filtered off with suction
  3. customthe DMF was removed in vacuo
  4. customCrystals of the title compound separated out
  5. washthese were washed with water, methanol and ether
  6. customdried

출처 및 근거

ORD 기록
ord-934a558e455a4a6d9a5a76c76274324d
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04762848

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