Pyridine → HCID 58455273、化合物

HRID 41821

反応式

HRID 41821 の反応式
[Cl:1][C:2](Cl)([O:4]C(=O)OC(Cl)(Cl)Cl)Cl.[CH2:13]1[O:18][CH:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[O:16][CH2:15][CH:14]1[OH:25].N1C=CC=CC=1>C(Cl)Cl>[C:2]([Cl:1])(=[O:4])[O:25][CH:14]1[CH2:13][O:18][CH:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[O:16][CH2:15]1

参加物

5

反応物 3

HCID 1049PyridineHCID 743621,3-Dioxan-5-ol, 2-phenyl-HCID 94429Triphosgene2 回

生成物 1

HCID 58455273HCID 58455273、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-40 °C

実験手順

Triphosgene (bis(trichloromethyl)carbonate (13.35 g, 45.0 mmol) was added under argon at room temperature to a solution of 1,3-O-benzylideneglycerol (18.02 g, 100.0 mmol) in dry CH2Cl2 (300 ml). The reaction mixture was cooled to −40° C. and a solution of pyridine (10.9 ml, 135.0 mmol) was added over 35 min under stirring. Upon completion of the addition the reaction mixture was stirred for 30 min at −40° C. Then it was allowed to warm to 0° C. over 60 min and subsequently warmed to rt over 3.5 h under stirring. The reaction product was used in the next step without any further purification

後処理

  1. additionUpon completion of the addition the reaction mixture
  2. stirringwas stirred for 30 min at −40° C
  3. temperatureto warm to 0° C. over 60 min
  4. temperaturesubsequently warmed to rt over 3.5 h
  5. stirringunder stirring
  6. customThe reaction product was used in the next step without any further purification

出典と根拠

ORDレコード
ord-88743db5226e4fbcacc170e4ad06550f
出典データセット
uspto-grants-2013_09
特許番号
US08535655B2

関連ノート

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