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Triethylamine → HCID 86621214、化合物

HRID 1855240
ノート
印刷プレビュー

反応式

HRID 1855240 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]3([C:13]([OH:15])=O)[CH2:12][CH2:11]3)=[CH:9][C:4]=2[O:3][CH2:2]1.O=S(Cl)Cl.[NH2:20][C:21]1[S:22][C:23]([CH:27]([C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=2[Cl:41])[NH:28][S@@:29]([C:31]([CH3:34])([CH3:33])[CH3:32])=[O:30])=[C:24]([CH3:26])[N:25]=1.CCN(CC)CC>CN(C=O)C.C(Cl)Cl>[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]3([C:13]([NH:20][C:21]4[S:22][C:23]([CH:27]([C:35]5[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=5[Cl:41])[NH:28][S@@:29]([C:31]([CH3:34])([CH3:32])[CH3:33])=[O:30])=[C:24]([CH3:26])[N:25]=4)=[O:15])[CH2:11][CH2:12]3)=[CH:9][C:4]=2[O:3][CH2:2]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 143496081-(1,3-Dioxaindan-5-yl)cyclopropane-1-carboxylic acidHCID 86621215(R)-N-((2-amino-4-methylthiazol-5-yl)(2-chlorophenyl)methyl)-2-methylpropane-2-sulfinamide

生成物 1

HCID 86621214HCID 86621214、化合物

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
触媒
HCID 6344Dichloromethane溶媒2 回

反応条件

温度
60 °C

実験手順

To 1-(benzo[d][1,3]dioxol-5-yl)cyclopropanecarboxylic acid (864 mg, 4.2 mmol) was slowly added SOCl2 (916 μL, 12.6 mmol) followed by DMF (3 drops). The reaction mixture was heated at 60° C. for 0.5 h. The excess SOCl2 was removed under vacuum. The acid chloride was then dissolved in anhydrous CH2Cl2 (6 mL) and was slowly added to a solution of (R)-N-((2-amino-4-methylthiazol-5-yl)(2-chlorophenyl)methyl)-2-methylpropane-2-sulfinamide (Isomer A) (1.35 g, 3.8 mmol) and Et3N (2.92 mL, 21.0 mmol) in anhydrous CH2Cl2 (18 mL). The reaction mixture was stirred at room temperature for 18 h, diluted with CH2Cl2 and washed with 1N HCl solution, saturated aqueous NaHCO3 solution and brine. The organic layer was dried over MgSO4 and concentrated to provide 1-(benzo[d][1,3]dioxol-5-yl)-N-(5-((2-chlorophenyl)((R)-1,1-dimethylethylsulfinamido)methyl)-4-methylthiazol-2-yl)cyclopropanecarboxamide (Isomer A) as an orange solid (1.54 g, 75%) that was used without further purification. HPLC ret. time 3.59 min, 10-99% CH3CN, 5 min run; ESI-MS 546.5 m/z (MH+).

後処理

  1. customThe excess SOCl2 was removed under vacuum
  2. dissolutionThe acid chloride was then dissolved in anhydrous CH2Cl2 (6 mL)
  3. washwashed with 1N HCl solution, saturated aqueous NaHCO3 solution and brine
  4. dry with materialThe organic layer was dried over MgSO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-7a415fe6d64447fbb37d1cc4e553585c
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08962856B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート