ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Sodium hydride → 1-t-butoxycarbonyl-4-(1-(4,4,4-trifluorobutyl)-1H-benzimidazol-2-yl)[1,4]diazepane

HRID 1584478
ノート
印刷プレビュー

反応式

HRID 1584478 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[NH:19][C:18]3[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=3[N:16]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].I[CH2:27][CH2:28][CH2:29][C:30]([F:33])([F:32])[F:31].[Cl-].[NH4+]>O1CCCC1.CN(C)C=O.C(OCC)(=O)C.CCCCCC>[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[N:16]([CH2:27][CH2:28][CH2:29][C:30]([F:33])([F:32])[F:31])[C:17]3[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=3[N:19]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 27751891,1,1-Trifluoro-4-iodobutaneHCID 184646551-t-butoxycarbonyl-4-(1H-benzimidazol-2-yl)[1,4]diazepane

生成物 1

HCID 212236081-t-butoxycarbonyl-4-(1-(4,4,4-trifluorobutyl)-1H-benzimidazol-2-yl)[1,4]diazepane

試薬・触媒・溶媒 3

HCID 6228
Dimethylformamide
溶媒
HCID 8028Tetrahydrofuran溶媒
HCID 21226206Ethyl acetate hexane溶媒

実験手順

Combine 1-t-butoxycarbonyl-4-(1H-benzimidazol-2-yl)[1,4]diazepane (1.5 g, 4.74 mmol) in tetrahydrofuran (45 mL) and dimethylformamide (5 mL). Cool in an ice bath. Add sodium hydride (0.23 g, 60% in oil, 5.7 mmol). Warm to ambient temperature. After about 90 minutes, when the gas evolution ceases, add 1-iodo-4,4,4-trifluorobutane (1.35 g, 5.7 mmol). After 18 hours, add ice and then a saturated aqueous solution of ammonium chloride. Evaporate the reaction mixture to remove most of the tetrahydrofuran, dilute with ethyl acetate and extract with water and then brine. Dry the organic layer over MgSO4, filter, and evaporate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with 60% ethyl acetate/hexane to give 1-t-butoxycarbonyl-4-(1-(4,4,4-trifluorobutyl)-1H-benzimidazol-2-yl)[1,4]diazepane: Rf =0.40 (silica gel, ethyl acetate).

後処理

  1. temperatureCool in an ice bath
  2. waitAfter 18 hours
  3. additionadd ice
  4. customEvaporate the reaction mixture
  5. customto remove most of the tetrahydrofuran
  6. additiondilute with ethyl acetate
  7. extractionextract with water
  8. dry with materialDry the organic layer over MgSO4
  9. filtrationfilter
  10. customevaporate in vacuo
  11. customto give a residue

出典と根拠

ORDレコード
ord-2ea7bcc5931b420bbd68169d7c70a9ef
出典データセット
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05932571

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート