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Formic Acid → (9aS)-8-azetidin-3-ylhexahydropyrazino[2,1-c][1,4]oxazin-4(3H)-one

HRID 2063319
ノート
印刷プレビュー

反応式

HRID 2063319 の反応式
C1(C(C2C=CC=CC=2)[N:8]2[CH2:11][CH:10]([N:12]3[CH2:21][CH2:20][N:19]4[C@H:14]([CH2:15][O:16][CH2:17][C:18]4=[O:22])[CH2:13]3)[CH2:9]2)C=CC=CC=1.C(O)=O.C([O-])=O.[NH4+]>C(O)C.[Pd]>[NH:8]1[CH2:11][CH:10]([N:12]2[CH2:21][CH2:20][N:19]3[C@H:14]([CH2:15][O:16][CH2:17][C:18]3=[O:22])[CH2:13]2)[CH2:9]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

6

反応物 3

HCID 284Formic AcidHCID 2723923Ammonium formateHCID 16124478(9aS)-8-[1-(diphenylmethyl)azetidin-3-yl]hexahydropyrazino-[2,1-c][1,4]oxazin-4(3H)-one

生成物 1

HCID 16124476(9aS)-8-azetidin-3-ylhexahydropyrazino[2,1-c][1,4]oxazin-4(3H)-one

試薬・触媒・溶媒 2

HCID 23938Palladium触媒
HCID 702
Ethanol
溶媒
2 回

反応条件

温度
120 °C

実験手順

(9aS)-8-[1-(Diphenylmethyl)azetidin-3-yl]hexahydropyrazino-[2,1-c][1,4]oxazin-4(3H)-one (85 mg, 0.22 mmol) was dissolved in ethanol (18 mL). The solution was transferred to a 25 mL vial, which contained ethanol (2 mL), 10% palladium on carbon (0.1 g), formic acid (0.1 g, 2.2 mmol) and ammonium formate (0.2 g, 3.17 mmol). The mixture was heated for 5 min at 120° C. using microwave single node heating. The catalyst was filtered off and the solution of crude (9aS)-8-azetidin-3-ylhexahydropyrazino[2,1-c][1,4]oxazin-4(3H)-one was used in the next step without purification and quantification.

後処理

  1. temperatureheating
  2. filtrationThe catalyst was filtered off
  3. customthe solution of crude (9aS)-8-azetidin-3-ylhexahydropyrazino[2,1-c][1,4]oxazin-4(3H)-one was used in the next step without purification and quantification

出典と根拠

ORDレコード
ord-02720b6636034bc5a193337f120f8bf1
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08288370B2

反応ノート

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