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Hydrochloric Acid → 3-[(1-Naphthyloxy)methyl]pyrrolidine

HRID 2242943
ノート
印刷プレビュー

反応式

HRID 2242943 の反応式
[C:1]1([O:11][CH2:12][CH:13]2[CH2:17][CH2:16][N:15](C(OC(C)(C)C)=O)[CH2:14]2)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.Cl>O1CCOCC1>[C:1]1([O:11][CH2:12][CH:13]2[CH2:17][CH2:16][NH:15][CH2:14]2)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 674164501,1-Dimethylethyl 3-[(1-naphthalenyloxy)methyl]-1-pyrrolidinecarboxylate

生成物 1

HCID 450755773-[(1-Naphthyloxy)methyl]pyrrolidine収率 72.2%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A solution of 0.42 g (1.28 mmol) of 1,1-dimethylethyl 3-[(1-naphthalenyloxy)methyl]-1-pyrrolidinecarboxylate, prepared in Step 12.1, in 10 ml of 1,4-dioxane and 6 ml of a 2N solution of aqueous hydrochloric acid is stirred for 6 hours. It is evaporated to dryness and then coevaporation is carried out twice with toluene. The solid residue is washed with diethyl ether. The solid is taken up in dichloromethane and concentrated ammonia solution is added until a basic pH is obtained. The system is filtered on a Whatman PTFE cartridge and the organic phase is concentrated, to give 0.21 g of oily product, which is used as it is in the following step.

後処理

  1. customIt is evaporated to dryness
  2. washThe solid residue is washed with diethyl ether
  3. additionconcentrated ammonia solution is added until a basic pH
  4. customis obtained
  5. filtrationThe system is filtered on a Whatman PTFE cartridge
  6. concentrationthe organic phase is concentrated

出典と根拠

ORDレコード
ord-ac6afefcd71e4832b9bbaecc7e3270dc
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07674805B2

反応ノート

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