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1-Isopropylhydrazine hydrochloride → {2-[4-[1,3]Dioxolan-2-ylmethyl-5-(4-fluoro-phenyl)-1-isopropyl-1H-pyrazol-3-yl]-ethyl}-carbamic acid benzyl ester

HRID 606621
ノート
印刷プレビュー

反応式

HRID 606621 の反応式
Cl.[CH:2]([NH:5][NH2:6])([CH3:4])[CH3:3].[CH2:7]([O:14][C:15](=[O:21])[NH:16][CH2:17][CH2:18][CH:19]=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[F:22][C:23]1[CH:28]=[CH:27][C:26]([CH:29]=[C:30]([N+]([O-])=O)[CH2:31][CH:32]2[O:36][CH2:35][CH2:34][O:33]2)=[CH:25][CH:24]=1>CCN(CC)CC>[CH2:7]([O:14][C:15](=[O:21])[NH:16][CH2:17][CH2:18][C:19]1[C:30]([CH2:31][CH:32]2[O:36][CH2:35][CH2:34][O:33]2)=[C:29]([C:26]2[CH:27]=[CH:28][C:23]([F:22])=[CH:24][CH:25]=2)[N:5]([CH:2]([CH3:4])[CH3:3])[N:6]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 855731-Isopropylhydrazine hydrochlorideHCID 10398106Benzyl (3-Oxopropyl)carbamateHCID 67047481HCID 67047481、化合物

生成物 1

HCID 54754013{2-[4-[1,3]Dioxolan-2-ylmethyl-5-(4-fluoro-phenyl)-1-isopropyl-1H-pyrazol-3-yl]-ethyl}-carbamic acid benzyl ester

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

A solution of isopropylhydrazine hydrochloride (1.07 g, 9.7 mmol) and (3-oxo-propyl)-carbamic acid benzyl ester (2.0 g, 9.7 mmol) in Et3N (20 mL) was heated at 60° C. After 1 h, 2-[3-(4-fluoro-phenyl)-2-nitro-allyl]-[1,3]dioxolane (2.2 g, 8.7 mmol) was added. After 16 h at 60° C., the mixture was cooled to rt and concentrated. The residue was partitioned between EtOAc and water. The organic layer was separated, dried (MgSO4), and concentrated. Purification by FCC gave the title compound.

後処理

  1. waitAfter 16 h at 60° C.
  2. concentrationconcentrated
  3. customThe residue was partitioned between EtOAc and water
  4. customThe organic layer was separated
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customPurification by FCC

出典と根拠

ORDレコード
ord-6649126592ae4aaabd70aa54307bddf2
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07915404B2

反応ノート

読み込み中…

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