Diisopropylethylamine → HCID 86762365、化合物

HRID 2367928ノート

反応式

HRID 2367928 の反応式
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:10]=[C:11]([C:15]2[N:20]=[C:19]([C:21]([O:23][CH3:24])=[O:22])[CH:18]=[CH:17][CH:16]=2)[CH:12]=[CH:13][CH:14]=1.[Cl:25][C:26](Cl)([O:28]C(=O)OC(Cl)(Cl)Cl)Cl.CCN(C(C)C)C(C)C>C(OCC)(=O)C>[Cl:25][C:26]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:10]=[C:11]([C:15]2[N:20]=[C:19]([C:21]([O:23][CH3:24])=[O:22])[CH:18]=[CH:17][CH:16]=2)[CH:12]=[CH:13][CH:14]=1)=[O:28]

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 94429TriphosgeneHCID 66815740HCID 66815740、化合物

生成物 1

HCID 86762365HCID 86762365、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a solution of methyl 6-(3-(6-hydroxyhexyloxy)phenyl)picolinate (13), (33 mg, 0.10 mmol, 1 eq.) in ethyl acetate (1 mL) was added triphosgene (14 mg, 0.047 mmol, 1.4 eq) dissolved in a minimum amount of ethyl acetate, followed immediately by DIEA (26 μL, 20 mg, 0.15 mmol, 1.5 eq). The mixture was stirred at room temperature for 30 min, the precipitated DIEA hydrochloride was filtered off, and the filtrate evaporated to dryness in vacuo. The oily residue of crude 14 was used directly for the next step.

後処理

  1. filtrationthe precipitated DIEA hydrochloride was filtered off
  2. customthe filtrate evaporated to dryness in vacuo

出典と根拠

ORDレコード
ord-f8c69387cab444e196d5b49cd848555c
出典データセット
uspto-grants-2014_04
特許番号
US08703700B2

反応ノート

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