N,N,N',N'-Tetramethylmethanediamine → 2-Dimethylaminomethyl-5-trifluoromethoxy-indan-1-one hydrochloride

HRID 2060070ノート

反応式

HRID 2060070 の反応式
[CH3:1][N:2]([CH2:4]N(C)C)[CH3:3].[F:8][C:9]([F:22])([F:21])[O:10][C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[C:16](=[O:20])[CH2:15][CH2:14]2.C([Cl:26])(=O)C>C(#N)C>[ClH:26].[CH3:1][N:2]([CH2:4][CH:15]1[CH2:14][C:13]2[C:17](=[CH:18][CH:19]=[C:11]([O:10][C:9]([F:22])([F:8])[F:21])[CH:12]=2)[C:16]1=[O:20])[CH3:3]

参加物

5

反応物 3

HCID 5829N,N,N',N'-TetramethylmethanediamineHCID 6367Acetyl chlorideHCID 221190265-(Trifluoromethoxy)-2,3-dihydro-1H-inden-1-one

生成物 1

HCID 694507812-Dimethylaminomethyl-5-trifluoromethoxy-indan-1-one hydrochloride

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

6.4 ml of bis-(dimethylamino)-methane were added to a solution of 10.1 g of the product from step 2 in 37 ml of acetonitrile; 3.3 ml of acetic acid chloride were added dropwise at from 0 to 10° C., a further 25 ml of acetonitrile were added, and stirring was carried out for 3 hours at 50° C. and then for 18 hours at room temperature. The resulting solid was filtered off with suction, washed twice with diethyl ether and dried in vacuo (yield 12.4 g).

後処理

  1. waitfor 18 hours at room temperature
  2. filtrationThe resulting solid was filtered off with suction
  3. washwashed twice with diethyl ether
  4. customdried in vacuo (yield 12.4 g)

出典と根拠

ORDレコード
ord-cc2de47fedfc49518a008117ab77328c
出典データセット
uspto-grants-2012_10
特許番号
US08278338B2

反応ノート

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