Potassium Iodide → HCID 20360368, 화합물

HRID 2082677노트

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HRID 2082677 반응식
Cl.Cl[CH2:3][CH2:4][NH:5][CH:6]([C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=1)[C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=1.[Cl:21][C:22]1[CH:37]=[CH:36][C:25]2[N:26]([CH:30]3[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]3)[C:27](=[O:29])[NH:28][C:24]=2[CH:23]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>O.CC(C)CC(=O)C>[F:13][C:10]1[CH:11]=[CH:12][C:7]([CH:6]([NH:5][CH2:4][CH2:3][N:33]2[CH2:32][CH2:31][CH:30]([N:26]3[C:25]4[CH:36]=[CH:37][C:22]([Cl:21])=[CH:23][C:24]=4[NH:28][C:27]3=[O:29])[CH2:35][CH2:34]2)[C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][CH:15]=2)=[CH:8][CH:9]=1

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 1046075-Chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-oneHCID 3017749N-[Bis(4-fluorophenyl)methyl]-2-chloroethan-1-amine--hydrogen chloride (1/1)

생성물 1

HCID 20360368HCID 20360368, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 7909Methyl Isobutyl Ketone용매

실험 절차

A mixture of 10 parts of N-(2-chloroethyl)-4-fluoro-α-(4-fluorophenyl)benzenemethanamine hydrochloride, 7.3 parts of 5-chloro-1,3-dihydro-1-(4-piperidinyl)-2H-benzimidazol-2-one, 10.6 parts of sodium carbonate, 0.1 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. Water is added to the reaction mixture. The precipitated product is filtered off and set aside. From the filtrate, the organic phase is separated, washed with water, dried, filtered and evaporated. The residue is stirred in 4-methyl-2-pentanone. The solid product is filtered off, combined with the precipitated product, obtained above, and crystallized from 4-methyl-2-pentanone. The product is filtered off and dried in vacuo at 95° C, yielding 5 parts of 1-{1-[2-{[bis(4-fluorophenyl)methyl]amino}ethyl]-4-piperidinyl}-5-chloro-1,3-dihydro-2H-benzimidazol-2-one; mp. 198.6° C.

후처리

  1. temperaturerefluxed overnight
  2. filtrationThe precipitated product is filtered off
  3. customFrom the filtrate, the organic phase is separated
  4. washwashed with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. stirringThe residue is stirred in 4-methyl-2-pentanone
  9. filtrationThe solid product is filtered off
  10. customobtained above, and
  11. customcrystallized from 4-methyl-2-pentanone
  12. filtrationThe product is filtered off
  13. customdried in vacuo at 95° C

출처 및 근거

ORD 기록
ord-d7bf29c4a1b442038f67a63a33954eef
출처 데이터셋
uspto-grants-1978_04
특허 번호
US04082755

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