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Ammonia → 4-Butoxymethyl-benzylamine

HRID 640151
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HRID 640151 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([O:11][CH2:12][C:13]1[CH:20]=[CH:19][C:16]([C:17]#[N:18])=[CH:15][CH:14]=1)[CH2:8][CH2:9][CH3:10].N>O1CCCC1>[CH2:7]([O:11][CH2:12][C:13]1[CH:14]=[CH:15][C:16]([CH2:17][NH2:18])=[CH:19][CH:20]=1)[CH2:8][CH2:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 21226445Aluminium lithium hydrideHCID 432676834-Butoxymethyl-benzonitrile

생성물 1

HCID 432675904-Butoxymethyl-benzylamine수율 101%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a mixture of lithium aluminum hydride (600 mg, 13 mmol, purity: 80%) and tetrahydrofuran (10 mL) was added a mixture of 4-butoxymethyl-benzonitrile (600 mg, 3.2 mmol) described in Manufacturing Example 33-1-1 and tetrahydrofuran (10 mL) at 0° C., which was stirred for 4 hours at room temperature. 28% Aqueous ammonia solution was added dropwise to the reaction mixture at 0° C. The reaction mixture was warmed to room temperature and filtered. The filtrate was concentrated under a reduced pressure to obtain the title compound (620 mg, 101%) as a crude product.

후처리

  1. additionwas added
  2. temperatureThe reaction mixture was warmed to room temperature
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated under a reduced pressure

출처 및 근거

ORD 기록
ord-b1d8dde2c8df4c88b02f2da828d4ca0d
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691882B2

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