Chloroform → HCID 131710452、化合物

HRID 1576486ノート

反応式

HRID 1576486 の反応式
[OH:1][C:2]1([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][C:10]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[NH:12][CH:11]=2)[CH2:4][CH2:3]1.[C:25](Cl)(=[O:28])[CH2:26][CH3:27].C(=O)([O-])[O-].[K+].[K+].C(Cl)(Cl)Cl>O>[C:19]1([C:2]2([O:1][C:25](=[O:28])[CH2:26][CH3:27])[CH2:3][CH2:4][N:5]([CH2:8][CH2:9][C:10]3[C:18]4[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=4)[NH:12][CH:11]=3)[CH2:6][CH2:7]2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

参加物

6

反応物 4

HCID 6212ChloroformHCID 11430Potassium CarbonateHCID 62324Propionyl chloride2 回HCID 12589402HCID 12589402、化合物

生成物 1

HCID 131710452HCID 131710452、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 4 g. (0.0125 mole) of 3-[2-(4-hydroxy-4-phenylpiperidinyl)ethyl]indole, 1.19 g. (0.0125 mole) of propionyl chloride and 7 g. of potassium carbonate in 50 ml. of chloroform was allowed to stir for 2 hours. Then 0.4 g. of additional propionyl chloride was added and allowed to stir another 30 minutes. The mixture was treated with 50 ml. of water and allowed to stir 30 minutes. The chloroform layer was separated, dried over magnesium sulfate and evaporated under reduced pressure to an oil. The oil was crystallized from benzene-isooctane and yielded 3.0 g. (64%) of product which melted at 140°-142° C. After an additional recrystallization the analytical sample melted at 142°-144° C.

後処理

  1. additionA mixture of 4 g
  2. stirringto stir another 30 minutes
  3. additionThe mixture was treated with 50 ml
  4. stirringto stir 30 minutes
  5. customThe chloroform layer was separated
  6. dry with materialdried over magnesium sulfate
  7. customevaporated under reduced pressure to an oil
  8. customThe oil was crystallized from benzene-isooctane
  9. customyielded 3.0 g
  10. customAfter an additional recrystallization the analytical sample melted at 142°-144° C.

出典と根拠

ORDレコード
ord-0a71f9ab643d4d6ca32f80bd7e77846d
出典データセット
uspto-grants-1976_09
特許番号
USRE028973

反応ノート

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