Hydrochloric Acid → HCID 12970145、化合物

HRID 458008ノート

反応式

HRID 458008 の反応式
CSC.B.[N+:5]([CH2:8][C:9]1([CH2:15][C:16]#[N:17])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)([O-:7])=[O:6].CO.Cl>C1(C)C=CC=CC=1.O1CCOCC1>[N+:5]([CH2:8][C:9]1([CH2:15][CH2:16][NH2:17])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1)([O-:7])=[O:6]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 11275397HCID 11275397、化合物HCID 12423031(Dimethyl sulfide)trihydroboron

生成物 1

HCID 12970145HCID 12970145、化合物収率 56.1%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

Borane methyl sulphide (2.0 M in toluene, 1.3 mL, 2.6 mmol) was added to compound 3 (0.4 g, 2.2 mmol) in toluene (10 mL) under nitrogen. After heating to 60° C. for 3 hours, the mixture was allowed to cool, and 15 mL methanol was added followed by 15 mL 4 M HCl in dioxane. After reflux for 1 hour, the mixture was evaporated to dryness. Crystallization from ethyl acetate gave the required product as colorless crystals (0.23 g, 47%); mp 170–173° C.

後処理

  1. temperatureto cool
  2. temperatureAfter reflux for 1 hour
  3. customthe mixture was evaporated to dryness
  4. customCrystallization from ethyl acetate

出典と根拠

ORDレコード
ord-7d4163abaf1641c888d8c2184146b26d
出典データセット
uspto-grants-2007_03
特許番号
US07189747B2

反応ノート

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