Potassium Iodide → HCID 20360368、化合物

HRID 2082677ノート

反応式

HRID 2082677 の反応式
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

参加物

7

反応物 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)

生成物 1

HCID 20360368HCID 20360368、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d7bf29c4a1b442038f67a63a33954eef
出典データセット
uspto-grants-1978_04
特許番号
US04082755

反応ノート

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