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

1,2-Dichloroethane → HCID 58537189、化合物

HRID 1804503
ノート
印刷プレビュー

反応式

HRID 1804503 の反応式
[CH2:1]([C:5]1[O:9][N:8]=[C:7]([C:10]([OH:12])=O)[C:6]=1[CH2:13][CH2:14][CH3:15])[CH:2]([CH3:4])[CH3:3].[CH2:16]([C:20]1[C:21]([C:28]([OH:30])=O)=[N:22][O:23][C:24]=1[CH2:25][CH2:26][CH3:27])[CH:17]([CH3:19])[CH3:18].O/[N:32]=[C:33](/[C:35]1[CH:52]=[CH:51][C:38]([CH2:39][N:40]2[CH2:43][CH:42]([C:44]([O:46][C:47]([CH3:50])([CH3:49])[CH3:48])=[O:45])[CH2:41]2)=[CH:37][CH:36]=1)\[NH2:34].C1C=CC2N(O)N=NC=2C=1.C(N(C(C)C)CC)(C)C.C(Cl)CCl>CN(C=O)C>[CH2:1]([C:5]1[O:9][N:8]=[C:7]([C:10]2[O:12][N:34]=[C:33]([C:35]3[CH:36]=[CH:37][C:38]([CH2:39][N:40]4[CH2:41][CH:42]([C:44]([O:46][C:47]([CH3:48])([CH3:50])[CH3:49])=[O:45])[CH2:43]4)=[CH:51][CH:52]=3)[N:32]=2)[C:6]=1[CH2:13][CH2:14][CH3:15])[CH:2]([CH3:3])[CH3:4].[CH2:16]([C:20]1[C:21]([C:28]2[O:30][N:34]=[C:33]([C:35]3[CH:36]=[CH:37][C:38]([CH2:39][N:40]4[CH2:41][CH:42]([C:44]([O:46][C:47]([CH3:48])([CH3:50])[CH3:49])=[O:45])[CH2:43]4)=[CH:51][CH:52]=3)[N:32]=2)=[N:22][O:23][C:24]=1[CH2:25][CH2:26][CH3:27])[CH:17]([CH3:18])[CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 58504340HCID 58504340、化合物HCID 58537221HCID 58537221、化合物HCID 58537233HCID 58537233、化合物

生成物 2

HCID 58537189
HCID 58537189、化合物
収率 66.6%
HCID 58537195HCID 58537195、化合物収率 66.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A mixture of 5-isobutyl-4-propylisoxazole-3-carboxylic acid, and 4-isobutyl-5-propylisoxazole-3-carboxylic acid (42.26 mg, 0.2 mmol), (Z)-tert-butyl 1-(4-(N′-hydroxycarbamimidoyl)benzyl)azetidine-3-carboxylate (61.1 mg, 0.200 mmol), HOBt (38.3 mg, 0.250 mmol), diisopropylethylamine (0.070 mL, 0.400 mmol) and EDC (47.9 mg, 0.250 mmol) in DMF (1 mL) was stirred at rt for 18 hr. DMF (1 mL) was added and the reaction mixture was warmed to 50° C. for 8 hr. The reaction mixture was partitioned between EtOAc (30 ml) and saturated sodium bicarbonate solution (30 ml). The organic layer was washed with water (2×30 ml) and brine (30 ml). After drying (MgSO4) and filtration, the organic layer was concentrated to afford an oil that was chromatographed on a 4 gm Isco silica gel cartridge, eluting with a 0-100% EtOAc/Hex gradient. The pure fractions were concentrated to afford a mixture of tert-butyl 1-(4-(5-(5-isobutyl-4-propylisoxazol-3-yl)-1,2,4-oxadiazol-3-yl)benzyl)azetidine-3-carboxylate (32 mg, 0.067 mmol, 66.6% yield) and tert-butyl 1-(4-(5-(4-isobutyl-5-propylisoxazol-3-yl)-1,2,4-oxadiazol-3-yl)benzyl)azetidine-3-carboxylate (32 mg, 0.067 mmol, 66.6% yield) as a colorless oil. HPLC retention time=1.89 minutes (YMC Combi 4.6×30 mm S-5 ODS column) eluting with 10-90% aqueous methanol+0.1 TFA a 2 minute gradient.

後処理

  1. temperaturethe reaction mixture was warmed to 50° C. for 8 hr
  2. customThe reaction mixture was partitioned between EtOAc (30 ml) and saturated sodium bicarbonate solution (30 ml)
  3. washThe organic layer was washed with water (2×30 ml) and brine (30 ml)
  4. customAfter drying
  5. filtration(MgSO4) and filtration
  6. concentrationthe organic layer was concentrated
  7. customto afford an oil that
  8. customwas chromatographed on a 4 gm Isco silica gel cartridge
  9. washeluting with a 0-100% EtOAc/Hex gradient
  10. concentrationThe pure fractions were concentrated
  11. customto afford

出典と根拠

ORDレコード
ord-9b36985d526f45f89c689d54dd4891b3
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08354398B2

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